HRID1027859

反应详情

EQUATION

反应方程式

HRID 1027859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

0.38 ml of 4N solution of hydrogen chloride in dioxane was added to 399 mg (1.50 mmol) of (RS)-S-(4-aminophenyl)-S-methyl-N-(trifluoroacetyl)sulfoximide and 404 mg (1.50 mmol) of (2R,3R)-3-(2-chloro-5-trifluoromethyl-pyrimidin-4-ylamino)-butan-2-ol in 7.3 ml acetonitrile and stirred for 9 hours at 60° C. The mixture was evaporated to dryness. 32.2 ml methanol and 1040 mg (7.50 mmol) of potassium carbonate were added and it was stirred for 1.5 hours at room temperature. It was diluted with saturated sodium chloride solution and was extracted with ethyl acetate (3×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. 565 mg (1.40 mmol) of the raw product was obtained.

WORKUP

后处理

  1. customThe mixture was evaporated to dryness
  2. stirringit was stirred for 1.5 hours at room temperature
  3. extractionwas extracted with ethyl acetate (3×)
  4. dry with materialThe combined organic phases were dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation