反应详情

温度

37 °C

6.0 mL Alcalase 2.4 L FG (Novozymes A/S; DK 2880 Bagsvaerd) was added to a warm solution (37° C.) of 7.2 g (40.4 mmol) Na2HPO4 dihydrate in 100 mL water and by the addition of NaH2PO4 dihydrate the pH was adjusted to 7.5. Then a solution of 5.5 g (19.2 mmol) methyl 2-acetylamino-3-(3-chloro-4-hydroxy-5-methyl-phenyl)-propionate in 50 mL acetone was added dropwise with stirring at 37° C. The pH value of the reaction mixture was kept constantly in the range from pH 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 exhaustively extracted with MTBE, the combined organic extracts were washed with 15% K2CO3 solution and dried over Na2SO4. After the desiccant and solvent had been eliminated the crude product (1.6 g) was further reacted without purification.

1. additionAfter the addition
2. stirringwas stirred for 4 h at 37° C
3. temperatureAfter cooling to RT the reaction mixture
4. extractionwas exhaustively extracted with MTBE
5. washthe combined organic extracts were washed with 15% K2CO3 solution
6. dry with materialdried over Na2SO4
7. customwas further reacted without purification