HRID561772

反应详情

EQUATION

反应方程式

HRID 561772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
87.5 °C

PROCEDURE

实验过程

A mixture consisting of methanesulfonamide (4.76 g) and 5-bromovaleric acid chloride (10 g) was heated at 85-90° C. for one hour, was cooled to room temperature, and was diluted with ethyl acetate (75 mL). The solution was washed with water, brine, and dried over sodium sulfate. The solution was filtered and evaporated to 40 mL of solvent, then cooled to −15° C. A white precipitate formed, which was collected by filtration to afford the title intermediate (11.4 g, 88%) as a white solid; melting point 98-100° C.

WORKUP

后处理

  1. temperaturewas cooled to room temperature
  2. washThe solution was washed with water, brine
  3. dry with materialdried over sodium sulfate
  4. filtrationThe solution was filtered
  5. customevaporated to 40 mL of solvent
  6. temperaturecooled to −15° C
  7. customA white precipitate formed
  8. filtrationwhich was collected by filtration