HRID1854784

反应详情

EQUATION

反应方程式

HRID 1854784 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 25 mL three neck flask with stirring arrangement, (1 gm) (R)-2,4-dichlorophenylethyl ammonium (S)-2-hydroxy-3-methoxy-3,3-diphenylpropionate and (0.726 gm) potassium tertiary butoxide (6.488 mmol) in 10 ml DMF at 25° C. were taken and stirred for 5 min. (0.604 gm) 4,6-dimethyl-2-(methylsulfonyl)pyrimidine (3.244 mmol) was added to the reaction mixture in one lot. The reaction mixture was stirred at room temperature for 6 hours and subsequently dumped into cold water and washed the aqueous layer with toluene. Aqueous layer was collected and acidified with HCl to pH 2. The solid was extracted with ethyl acetate, and wash the ethyl acetate layer with water followed by brine. Dry over sodium sulphate and concentrated on Buchi Rotavapor.

WORKUP

后处理

  1. additionwas added to the reaction mixture in one lot
  2. washwashed the aqueous layer with toluene
  3. customAqueous layer was collected
  4. extractionThe solid was extracted with ethyl acetate
  5. washwash the ethyl acetate layer with water
  6. dry with materialDry over sodium sulphate
  7. concentrationconcentrated on Buchi Rotavapor