280115-84-6|Methyl 4-((tert-butoxycarbonyl)amino)nicotinate| Ambeed

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CAS No. :	280115-84-6
Formula :	C₁₂H₁₆N₂O₄
M.W :	252.27
SMILES Code :	O=C(OC)C1=CN=CC=C1NC(OC(C)(C)C)=O
MDL No. :	MFCD19689618

Yield	Reaction Conditions	Operation in experiment
81%	In methanol; hexane; for 0.25h;	To a stirring suspension of4- (Boc-amino) pyridine-3- carboxylic acid (1.04 g, 4.37 mmol) in methanol (3.5 mL) was added a 2 M solution of (trimethylsilyl) diazomethane in hexanes (3.5 mL, 7 mmol). After 15 min, acetic acid was added and the solvents were removed in vacuo. The residue was chromatographed over silica gel, eluting with a step gradient of 20% ethyl acetate in hexanes through 70% ethyl acetate in hexanes. The product containing fractions were combined and concentrated in vacuo to give the title compound (0.894 g,81%) as a white solid. 1NMR
0.894 g (81%)	With acetic acid; In methanol; ethyl acetate;	C. Methyl 4-(Boc-amino)pyridine-3-carboxylate. To a stirring suspension of <strong>[171178-34-0]4-(Boc-amino)pyridine-3-carboxylic acid</strong> (1.04 g, 4.37 mmol) in methanol (3.5 mL) was added a 2 M solution of (trimethylsilyl)diazomethane in hexanes (3.5 mL, 7 mmol). After 15 min, acetic acid was added and the solvents were removed in vacuo. The residue was chromatographed over silica gel, eluding with a step gradient of 20 % ethyl acetate in hexanes through 70 % ethyl acetate in hexanes. The product containing fractions were combined and concentrated in vacuo to give 0.894 g (81%) of a white solid. 1H-NMR

Yield	Reaction Conditions	Operation in experiment
83%		4-tert-Butoxycarbonylamino-nicotinic acicL To a solution of 4-tert- butoxycarbonylamino-nicotinic acid methyl ester (6.02g, 23.86 mmol) in dioxane (100 mL) was added aq. sodium hydroxide (0.970 N solution, 28.05 mL, 27.20 mmol). The solution was heated to 6O0C for lhr then cooled. Aqueous hydrochloric acid (1.03 IM solution, 26.99mL, 27.20 mmol) was added and the mixture was extracted with chloroform (5x100 mL). The extracts were dried (MgSO4), filtered, and evaporated to give 4-tert-Butoxycarbonylamino-nicotinic acid, a cream solid (4.7Og, 83% yield).
		Example 12 SYNTHESIS of Compound 47 Preparation OF 4-TERT-BUTOXYCARBONYLAMINO-NICOTINIC acid : [0114] To A solution OF 4-TERT-BUTOXYCARBONYLAMINO-NICOTINIC acid methyl ester (6. 02g, 23. 86 MMOL) in dioxane (100 ML) was added AQ. sodium hydroxide (0. 970N solution, 28. 05mL, 27. 20 MMOL). The solution was heated to 60C for Ihr then cooled. Aqueous hydrochloric acid (1. 031M solution, 26. 99mL, 27. 20 mmol) was added and the mixture was extracted with chloroform (SIX100 ML). The extracts were dried (MGS04) and evaporated to give 4-TERT- BUTOXYCARBONYLAMINO-NICOTINIC acid, A cream solid (4. 70g, 83% yield) without further purification.

Precautionary Statements-General
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Prevention
Code	Phrase
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P222	Do not allow contact with air.
P223	Keep away from any possible contact with water, because of violent reaction and possible flash fire.
P230	Keep wetted
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P232	Protect from moisture.
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P234	Keep only in original container.
P235	Keep cool
P240	Ground/bond container and receiving equipment.
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P262	Do not get in eyes, on skin, or on clothing.
P263	Avoid contact during pregnancy/while nursing.
P264	Wash hands thoroughly after handling.
P265	Wash skin thouroughly after handling.
P270	Do not eat, drink or smoke when using this product.
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P272	Contaminated work clothing should not be allowed out of the workplace.
P273	Avoid release to the environment.
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P281	Use personal protective equipment as required.
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P284	Wear respiratory protection.
P285	In case of inadequate ventilation wear respiratory protection.
P231 + P232	Handle under inert gas. Protect from moisture.
P235 + P410	Keep cool. Protect from sunlight.
Response
Code	Phrase
P301	IF SWALLOWED:
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P305	IF IN EYES:
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P320
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P321
P322
P330	Rinse mouth.
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P341	If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P342	If experiencing respiratory symptoms:
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P370	In case of fire:
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P378
P380	Evacuate area.
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P390	Absorb spillage to prevent material damage.
P391	Collect spillage. Hazardous to the aquatic environment
P301 + P310	IF SWALLOWED: Immediately call a POISON CENTER or doctor/physician.
P301 + P312	IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell.
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P302 + P350	IF ON SKIN: Gently wash with plenty of soap and water.
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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.
P306 + P360	IF ON CLOTHING: Rinse Immediately contaminated CLOTHING and SKIN with plenty of water before removing clothes.
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.
P370 + P378	In case of fire:
P370 + P380	In case of fire: Evacuate area.
P370 + P380 + P375	In case of fire: Evacuate area. Fight fire remotely due to the risk of explosion.
P371 + P380 + P375	In case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion.
Storage
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P401
P402	Store in a dry place.
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P411 + P235	Keep cool.
Disposal
Code	Phrase
P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

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CAS No.: 280115-84-6

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CAS No.: 280115-84-6

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[ 280115-84-6 ] Synthesis Path-Upstream 1~1

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Physical hazards
Code	Phrase
H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
H203	Explosive; fire, blast or projection hazard
H204	Fire or projection hazard
H205	May mass explode in fire
H220	Extremely flammable gas
H221	Flammable gas
H222	Extremely flammable aerosol
H223	Flammable aerosol
H224	Extremely flammable liquid and vapour
H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
H227	Combustible liquid
H228	Flammable solid
H229	Pressurized container: may burst if heated
H230	May react explosively even in the absence of air
H231	May react explosively even in the absence of air at elevated pressure and/or temperature
H240	Heating may cause an explosion
H241	Heating may cause a fire or explosion
H242	Heating may cause a fire
H250	Catches fire spontaneously if exposed to air
H251	Self-heating; may catch fire
H252	Self-heating in large quantities; may catch fire
H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
H270	May cause or intensify fire; oxidizer
H271	May cause fire or explosion; strong oxidizer
H272	May intensify fire; oxidizer
H280	Contains gas under pressure; may explode if heated
H281	Contains refrigerated gas; may cause cryogenic burns or injury
H290	May be corrosive to metals
Health hazards
Code	Phrase
H300	Fatal if swallowed
H301	Toxic if swallowed
H302	Harmful if swallowed
H303	May be harmful if swallowed