[ CAS No. 1007112-35-7 ] {[proInfo.proName]}

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Quality Control of [ 1007112-35-7 ]

COA NMR CNMR HPLC LC-MS

Related Doc. of [ 1007112-35-7 ]

SDS Specification

Alternatived Products of [ 1007112-35-7 ]

Product Details of [ 1007112-35-7 ]

CAS No. :	1007112-35-7	MDL No. :	MFCD11111729
Formula :	C₉H₆ClNO₃	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	-
M.W :	211.60	Pubchem ID :	-
Synonyms :

Safety of [ 1007112-35-7 ]

Signal Word:		Class:
Precautionary Statements:		UN#:
Hazard Statements:		Packing Group:

Application In Synthesis of [ 1007112-35-7 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

Downstream synthetic route of [ 1007112-35-7 ]

[ 1007112-35-7 ] Synthesis Path-Downstream 1~11

1
[ 1007112-35-7 ]
[ 154634-96-5 ]
[ 1007112-69-7 ]

Yield	Reaction Conditions	Operation in experiment
89%	With potassium carbonate In N,N-dimethyl-formamide at 35℃; for 17h;	88.A Step A: A mixture of methyl 2-chlorobenzoxazole-4-carboxylate (620 mg, 2.96 mmol) and (3S,5S)-3,5-dimethylmorpholine (341 mg, 2.96 mmol) and potassium carbonate (1.0 g, 7.4 mmol), in DMF (15 mL), was stirred in a 35° C. oil bath. After 17 h, the reaction mixture was cooled to ambient temperature, diluted with H2O (50 mL) and extracted with EtOAc (2×30 mL). The combined organic layers were washed with H2O (3×20 mL), brine (20 mL), dried (Na2SO4), and concentrated under reduced pressure. Methyl 2-((3 S,5S)-3,5-dimethylmorpholino)benzoxazole-4-carboxylate (770 mg, 89%) was obtained as an amber oil. 1H NMR consistent.
	In tetrahydrofuran

Reference： [1]Current Patent Assignee: CURIA INC - US2008/255114, 2008, A1 Location in patent: Page/Page column 29-30
[2]Location in patent: scheme or table Yang, Zhicai; Fairfax, David J.; Maeng, Jun-Ho; Masih, Liaqat; Usyatinsky, Alexander; Hassler, Carla; Isaacson, Soshanna; Fitzpatrick, Kevin; Deorazio, Russell J.; Chen, Jianqing; Harding, James P.; Isherwood, Matthew; Dobritsa, Svetlana; Christensen, Kevin L.; Wierschke, Jonathan D.; Bliss, Brian I.; Peterson, Lisa H.; Beer, Cathy M.; Cioffi, Christopher; Lynch, Michael; Rennells, W. Martin; Richards, Justin J.; Rust, Timothy; Khmelnitsky, Yuri L.; Cohen, Marlene L.; Manning, David D. [Bioorganic and Medicinal Chemistry Letters, 2010, vol. 20, # 22, p. 6538 - 6541]

2
[ 1007112-35-7 ]
[ 91476-80-1 ]
[ 1007112-77-7 ]

Yield	Reaction Conditions	Operation in experiment
37%		Step A: To a solution of NaH (60% dispersion in mineral oil, 0.130 g, 3.25 mmol) in THF (10 mL) was added <strong>[91476-80-1]5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine</strong> (0.33 g, 2.71 mmol) and the reaction mixture stirred for 10 min. Methyl 2-chlorobenzoxazole-4-carboxylate (478 mg, 2.26 mmol), in THF (10 mL) was added and the reaction mixture was allowed to stir at room temperature 17 h. The reaction mixture was quenched with CH3OH (3 mL), and adsorbed onto silica gel (2 g). The crude product was purified by column chromatography (silica gel, 0.5 to 10% CH3OH in CH2Cl2) to afford methyl 2-(5,6-dihydroimidazo[1,2-a]pyrazin-7(8H)-yl)benzoxazole-4-carboxylate (251 mg, 37%) as an orange oil. 1H NMR and MS consistent.

Reference： [1]Patent: US2008/255114,2008,A1 .Location in patent: Page/Page column 26

3
[ 324748-62-1 ]
[ 1007112-35-7 ]
[ 1007112-70-0 ]

Yield	Reaction Conditions	Operation in experiment
54%	Stage #1: (S)-1-benzyl-3-isopropylpiperazine With sodium hydride In 1,2-dimethoxyethane at 20℃; for 1h; Stage #2: 2-chloro-benzooxazole-4-carboxylic acid methyl ester In 1,2-dimethoxyethane at 20℃; for 17h;	76.A Step A: To a solution of (2S)-4-benzyl-2-isopropylpiperazine (363 mg, 1.66 mmol) in 1,2-dimethoxyethane (10 mL) at room temperature, was added NaH (80 mg, 1.66 mmol, 60% suspension in mineral oil) and the mixture was stirred for 1 h. Methyl 2-chlorobenzoxazole-4-carboxylate (351 mg, 1.66 mmol) was added to the reaction mixture and the reaction was stirred at room temperature for 17 h. The reaction mixture was quenched with CH3OH (10 mL), silica gel (15 mL) was added, and solvent removed under reduced pressure. The mixture was purified by column chromatography (silica gel, 0 to 100% EtOAc in hexanes) to afford (S)-methyl 2-(4-benzyl-2-isopropylpiperazin-1-yl)benzoxazole-4-carboxylate (355 mg, 54%) as a pale yellow oil. MS consistent.

Reference： [1]Current Patent Assignee: CURIA INC - US2008/255114, 2008, A1 Location in patent: Page/Page column 25

4
[ 1007112-35-7 ]
[ 120737-78-2 ]
[ 1007112-87-9 ]

Yield	Reaction Conditions	Operation in experiment
63%		Step A: To a solution of <strong>[120737-78-2]tert-butyl 2-methylpiperazine-1-carboxylate</strong> (340 mg, 1.70 mmol) in THF (5 mL) was added sodium hydride (60%, 82 mg, 2.04 mmol). The reaction mixture was stirred at room temperature for 5 min, then methyl 2-chlorobenzoxazole-4-carboxylate (300 mg, 1.41 mmol) in THF (5 mL) was added to the reaction mixture. The reaction mixture was stirred at room temperature for 19 h. The mixture was concentrated under reduced pressure and the resulting residue was purified by column chromatography (silica gel, 20% EtOAc in hexane) to afford methyl 2-(4-(tert-butoxycarbonyl)-3-methylpiperazin-1-yl)benzoxazole-4-carboxylate (336 mg, 63%) as yellow solid. MS consistent.

Reference： [1]Patent: US2008/255114,2008,A1 .Location in patent: Page/Page column 32

5
[ 1007112-35-7 ]
[ 154634-96-5 ]
[ 1007112-69-7 ]
[ 100246-04-6 ]

Yield	Reaction Conditions	Operation in experiment
	Stage #1: (+)-(S,S)-3,5-dimethylmorpholine With sodium hydride In 1,2-dimethoxyethane for 0.166667h; Stage #2: 2-chloro-benzooxazole-4-carboxylic acid methyl ester In 1,2-dimethoxyethane at 0 - 20℃; for 72h;	75.A Step A: To a solution of (3S,5S)-dimethylmorpholine (209 mg, 1.82 mmol) in 1,2-dimethoxyethane (10 mL) was added NaH(60% suspension in mineral oil, 146 mg, 3.64 mmol). After 10 min the reaction mixture was cooled to 0° C. and methyl 2-chlorobenzoxazole-4-carboxylate (500 mg, 2.36 mmol) was added portion-wise over 5 min. After 10 min, the reaction mixture was warmed to ambient temperature and allowed to stir for 3 days. The reaction mixture was quenched with CH3OH (10 mL) and then dry loaded onto silica gel (4.5 g). Purification by chromatography (silica gel, 0 to 20% EtOAc in hexanes) gave a 1:1 mixture of methyl 2-((3S,5S)-3,5-dimethylmorpholino)benzoxazole-4-carboxylate and methyl 2-oxo-2,3-dihydrobenzoxazole-4-carboxylate (312 mg, 59%) as an off-white solid. MS consistent.

Reference： [1]Current Patent Assignee: CURIA INC - US2008/255114, 2008, A1 Location in patent: Page/Page column 25

6
[ 674792-05-3 ]
[ 1007112-35-7 ]
[ 1007112-76-6 ]

Yield	Reaction Conditions	Operation in experiment
39%		Step A: To a solution of <strong>[674792-05-3]1-tert-butyloxycarbonyl-(S)-2-isopropylpiperazine</strong> (384 mg, 1.7 mmol) in DME (10 mL) was added NaH (70 mg of 60% suspension in mineral oil, 1.6 mmol) and the mixture was stirred for 1 h at room temperature. Methyl 2-chlorobenzoxazole-4-carboxylate (368 mg, 1.6 mmol) was added to the reaction mixture and suspension formed was stirred at room temperature for 17 h. The reaction mixture was quenched with CH3OH (10 mL), silica gel (15 mL) was added, and solvent removed under reduced pressure. The mixture was purified by column chromatography (silica gel, 0 to 80% EtOAc in CH2Cl2) to afford methyl 2-(4-(tert-butoxycarbonyl)-(S)-3-isopropylpiperazin-1-yl)benzoxazole-4-carboxylate (255 mg, 39%) as a white foam. 1H NMR and MS consistent.

Reference： [1]Patent: US2008/255114,2008,A1 .Location in patent: Page/Page column 26

7
[ 674792-06-4 ]
[ 1007112-35-7 ]
[ 1007112-68-6 ]

Yield	Reaction Conditions	Operation in experiment
32%		Step A: To a solution of <strong>[674792-06-4]1-tert-butyloxycarbonyl-(2S)-2-isobutylpiperazine</strong> (384 mg, 1.6 mmol) in DME (10 mL) was added NaH (70 mg of 60% suspension in mineral oil, 1.6 mmol) and the mixture was stirred for 1 h at room temperature. Methyl 2-chlorobenzoxazole-4-carboxylate (368 mg, 1.6 mmol) was added to the reaction mixture and suspension formed was stirred at room temperature for 17 h. The reaction mixture was quenched with CH3OH (10 mL), silica gel (15 mL) was added, and solvent removed under reduced pressure. The mixture was purified by column chromatography ((silica gel, 0 to 80% EtOAc in CH2Cl2) to afford methyl 2-(4-(tert-butoxycarbonyl)-(3S)-3-isobutylpiperazine-1-yl)benzoxazole-4-carboxylate (219 mg, 32%) as a clear oil: 1H NMR and MS consistent.

Reference： [1]Patent: US2008/255114,2008,A1 .Location in patent: Page/Page column 24

8
[ 4045-24-3 ]
[ 1007112-35-7 ]
[ 1007112-83-5 ]

Yield	Reaction Conditions	Operation in experiment
50%	With sodium hydride; In 1-methyl-pyrrolidin-2-one; at 20℃; for 18.0833h;	Step A: To a solution of methyl 2-chlorobenzoxazole-4-carboxylate (210 mg, 0.99 mmol) in NMP (5 mL) was added <strong>[4045-24-3]4-methoxypiperidine</strong> (230 mg, 1.98 mmol) in NMP (5 mL) at room temperature. NaH was added to the mixture in two portions in 5 min. The mixture was stirred at room temperature for 18 h. The reaction was quenched by adding 10 mL of CH3OH followed by concentration to dryness. The crude material was purified by column chromatography (silica gel, 50% EtOAc in hexane) to afford methyl 2-(4-methoxypiperidin-1-yl)benzoxazole-4-carboxylate (146 mg, 50%) as a yellow solid. MS consistent.

Reference： [1]Patent: US2008/255114,2008,A1 .Location in patent: Page/Page column 30

9
[ 748117-01-3 ]
[ 1007112-35-7 ]
[ 1014712-95-8 ]

Yield	Reaction Conditions	Operation in experiment
	In tetrahydrofuran

Reference： [1]Location in patent: scheme or table Yang, Zhicai; Fairfax, David J.; Maeng, Jun-Ho; Masih, Liaqat; Usyatinsky, Alexander; Hassler, Carla; Isaacson, Soshanna; Fitzpatrick, Kevin; Deorazio, Russell J.; Chen, Jianqing; Harding, James P.; Isherwood, Matthew; Dobritsa, Svetlana; Christensen, Kevin L.; Wierschke, Jonathan D.; Bliss, Brian I.; Peterson, Lisa H.; Beer, Cathy M.; Cioffi, Christopher; Lynch, Michael; Rennells, W. Martin; Richards, Justin J.; Rust, Timothy; Khmelnitsky, Yuri L.; Cohen, Marlene L.; Manning, David D. [Bioorganic and Medicinal Chemistry Letters, 2010, vol. 20, # 22, p. 6538 - 6541]

10
[ 77897-21-3 ]
[ 1007112-35-7 ]
[ 1014713-51-9 ]

Yield	Reaction Conditions	Operation in experiment
	In tetrahydrofuran

11
[ 77897-22-4 ]
[ 1007112-35-7 ]
[ 1014714-17-0 ]

Yield	Reaction Conditions	Operation in experiment
	In tetrahydrofuran

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P351	Rinse cautiously with water for several minutes.
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P353	Rinse skin with water/shower.
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P302 + P334	IF ON SKIN: Immerse in cool water/wrap in wet bandages.
P302 + P350	IF ON SKIN: Gently wash with plenty of soap and water.
P303 + P361 + P353	IF ON SKIN (or hair): Remove/Take off Immediately all contaminated clothing. Rinse SKIN with water/shower.
P304 + P312	IF INHALED: Call a POISON CENTER or doctor/physician if you feel unwell.
P304 + P340	IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
P304 + P341	IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P305 + P351 + P338	IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing.
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P307 + P311	IF exposed: call a POISON CENTER or doctor/physician.
P308 + P313	IF exposed or concerned: Get medical advice/attention.
P309 + P311	IF exposed or if you feel unwell: call a POISON CENTER or doctor/physician.
P332 + P313	IF SKIN irritation occurs: Get medical advice/attention.
P333 + P313	IF SKIN irritation or rash occurs: Get medical advice/attention.
P335 + P334	Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
P337 + P313	IF eye irritation persists: Get medical advice/attention.
P342 + P311	IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician.
P370 + P376	In case of fire: Stop leak if safe to Do so.
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H411	Toxic to aquatic life with long-lasting effects
H412	Harmful to aquatic life with long-lasting effects
H413	May cause long-lasting harmful effects to aquatic life
H420	Harms public health and the environment by destroying ozone in the upper atmosphere

[ CAS No. 1007112-35-7 ] {[proInfo.proName]}

Quality Control of [ 1007112-35-7 ]

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Safety of [ 1007112-35-7 ]

Application In Synthesis of [ 1007112-35-7 ]

[ 1007112-35-7 ] Synthesis Path-Downstream 1~11

Precautionary Statements-General

Prevention

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Storage

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Physical hazards

Health hazards

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