Acetyl chloride, 2-amino-2-oxo- synthesis

Yield:-

Reaction Conditions:

with thionyl chloride;N,N-dimethyl-formamide in dichloromethane; for 3 h;Reflux;

Steps:

b) Preparation of Oxalamides 93 and 98
2-Amino-2-Oxoacetyl Chloride RBO 56082

b) Preparation of Oxalamides 93 and 98
2-Amino-2-Oxoacetyl Chloride RBO 56082
To a solution of oxamic acid (500 mg, 5.61 mmol) in dry CH₂Cl₂ (20 mL) in a 50 mL round bottom flask equipped with a magnetic stirrer was added SOCl₂ (4.07 mL, 56.10 mmol) followed by 1 drop of DMF and the mixture was stirred under reflux for 3 h then cooled to 25° C. After concentration to dryness at 40° C. under vacuum, the residue was diluted with CH₂Cl₂ (20 mL) before concentration back to dryness (done twice), giving 633 mg of a pale yellow solid 2-amino-2-oxoacetyl chloride RBO 56082 that was used in the next step without further purification (quant. crude yield).

References:

US2015/158895,2015,A1 Location in patent:Paragraph 0389; 0390