HRID1887430

反应详情

EQUATION

反应方程式

HRID 1887430 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (0.19 ml) was added to a solution of the compound 5-1 synthesized from 7-fluorochroman-4-one according to Example 4 (200 mg) in tetrahydrofuran (3.0 ml), cooled in an ice bath. A solution of methanesulfonyl chloride (177 mg) in tetrahydrofuran (2.0 ml) was added dropwise at the same temperature, followed by stirring for 1.5 hours. After confirming disappearance of the raw material, the reaction mixture was added to aqueous sodium bicarbonate to terminate the reaction. The aqueous layer was extracted with ethyl acetate. The aqueous layer was further extracted with ethyl acetate, and the combined organic layers were dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to obtain the title compound (214 mg), which was used for the next reaction as a crude product.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. customto terminate
  3. customthe reaction
  4. extractionThe aqueous layer was extracted with ethyl acetate
  5. extractionThe aqueous layer was further extracted with ethyl acetate
  6. dry with materialthe combined organic layers were dried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure