46460-25-7|Ethyl 2-oxo-2-((pyridin-2-ylmethyl)amino)acetate| Ambeed

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CAS No. :	46460-25-7
Formula :	C₁₀H₁₂N₂O₃
M.W :	208.21
SMILES Code :	O=C(OCC)C(NCC1=NC=CC=C1)=O

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302-H315-H319
Precautionary Statements:	P501-P270-P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P312+P330

Yield	Reaction Conditions	Operation in experiment
70%	With phosphorus pentoxide; trichlorophosphate; at 110℃; for 5.0h;	A solution of ethyl [(pyridin-2-ylmethyl)carbamoyl]fonTlate (1.00 g, 4.80 mmol, 1.00 equiv) and phosphorus pentoxide (3.41 g, 24.02 mmol, 5.00 equiv) in phosphorus oxychloride (30 mL) was stirred for 5 h at 110 C. The resulting mixture was concentrated under vacuum. The residue waspurified by silica gel column chromatography eluting with ethyl acetate/petroleum ether (1:1). This resulted in 635 mg (70%) of the title compound as a yellow solid. LC-MS (ES, m/z): 191 [M+H] .
44%		A solution of ethyl oxo[(pyridin-2-ylmethyl)amino]acetate (40 g, 192 mmol) in POCl3 (300 mL) was heated to reflux for 18 h. The mixture was concentrated and saturated aqueous NaHCO3 was added. The mixture was extracted with EtOAc (3 x, 500 mL) and the combined organic extracts were washed with saturated brine, dried over Na2SO4, filtered, and concentrated to give a black oily solid. The residue was purified by silica gel chromatography (12%-70% EtOAc/Hexanes) to give the title compound (16 g, 44%). MS 191.1 (M + 1).
2.4 g	With pyridine; trifluoroacetic anhydride; In dichloromethane; at -15 - -10℃; for 12.0h;	2-(Aminomethyl)pyridine (1.5 g, 13.9 mmol) and pyridine (3.62 g, 45.8 mmol) were dissolved in CH2Cl2 (20 mL), and the solution was cooled by using an ice bath. A solution of ethyl oxalyl chloride (1.89 g, 13.9 mmol) in CH2Cl2 (10 mL) was added dropwise at 0 to -5 C. After addition, the mixture was stirred for 2 h and a solution of TFAA (3.06 g, 14.6 mmol) in CH2Cl2 (10 mL) was added dropwise at -15 to -10 C (ice-salt bath). The reaction mixture was allowed to stand overnight in the bath, then washed with sat. aq NaHCO3, and the CH2Cl2 layer was dried over Na2SO4 and concentrated. Yield: 2.4 g (91%); white solid; mp 80 C (Lit. [13] 80 C). The 1H and 13C NMR spectroscopic data were identical to those reported previously. [4,14,18]

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P378
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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:
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P371 + P380 + P375	In case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion.
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P411 + P235	Keep cool.
Disposal
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P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

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CAS No.: 46460-25-7

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CAS No.: 46460-25-7

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[ 46460-25-7 ] Synthesis Path-Downstream 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