Carbamic acid, (2,2,2-trifluoroethyl)-, 1,1-dimethylethyl ester (9CI) synthesis

Yield:470703-82-3 84.5%

Reaction Conditions:

with N-ethyl-N,N-diisopropylamine in dichloromethane; for 12 h;

Steps:

[00458] 2,2,2-trifluoroethan-1-amine (397 μL, 5.05 mmol) was diluted with DCM (30 mL) followed by the addition of DIEA (882 μL, 5.05 mmol) and di-tert-butyl dicarbonate (1102 mg, 5.05 mmol). After stirring for 12 hours, the reaction was diluted with DCM and water. The layers were separated and the ethyl acetate was dried over MgSO4, filtered and concentrated. The material was purified on silica gel (10-30% ethyl acetate/hexanes) to afford tert-butyl (2,2,2-trifluoroethyl)carbamate (850 mg, 4.27 mmol, 84.5 % yield).

References:

WO2019/113190,2019,A1 Location in patent:Paragraph 00458