Dichloromethane → HCID 86760963, compound

Participants

Reaction Conditions

Reaction Steps

4 mL Alcalase 2.4 L FG (Novozymes A/S; DK 2880 Bagsvaerd) was added to a solution of 3.65 g (20.5 mmol) Na2HPO4 dihydrate in 130 mL water warmed to 37° C. and the pH was adjusted to 7.5 by the addition of NaH2PO4 dihydrate. Then a solution of 3.8 g (9.84 mmol) ethyl 2-acetylamino-3-(4-amino-3,5-bis-trifluoromethyl-phenyl)-propionate in 40 mL acetone was added dropwise at 37° C. with stirring. The pH value of the reaction mixture was constantly kept in the range from 7.4-7.6 by the addition of 1 M NaOH. After the addition had ended the mixture was stirred for 4 h at 37° C. After cooling to RT the reaction mixture was combined with 300 mL DCM, 300 mL 15% K2CO3 solution and 200 mL water. The organic phase was separated off, washed with 7% K2CO3 solution and dried over Na2SO4. After the desiccant and solvent had been eliminated the crude product (2.2 g) was further reacted without purification. ESI-MS: (M+H)+387 Rf=0.60 (silica gel, PE/EtOAc 1:1)

Provenance & Evidence