HRID339888

反应详情

EQUATION

反应方程式

HRID 339888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 70 mg of 5-(4-bromophenyl)-2-methoxy-5,6,6-trimethyl-5,6-dihydro-1,4,3-oxathiazine 4,4-dioxide and 66 mg of (S)-3-(tert-butyldimethylsilanyloxy)-1-(2-fluorophenyl)propylamine in 1 ml of methylene chloride was stirred under a gentle argon stream, such that the solvent evaporated gradually. After stirring at room temperature overnight, the residue was dissolved in 20 ml of dichloromethane and extracted with 10 ml of 0.5 N aqueous hydrochloric acid and 10 ml of water. The organic phase was dried using a phase separator cartridge (Chromabond® PTS), concentrated by rotary evaporation and dried under high vacuum. This gave the product (113 mg) with a molecular weight of 613.7 g/mol (C27H38BrFN2O4SSi); MS (ESI): m/e=614 (M+H+).

WORKUP

后处理

  1. customevaporated gradually
  2. dissolutionthe residue was dissolved in 20 ml of dichloromethane
  3. extractionextracted with 10 ml of 0.5 N aqueous hydrochloric acid and 10 ml of water
  4. customThe organic phase was dried
  5. concentrationconcentrated by rotary evaporation
  6. customdried under high vacuum