HRID2036796

反应详情

EQUATION

反应方程式

HRID 2036796 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5-bromopyridine-3-sulfonyl chloride (3.5 g, 14 mmol) and glycine ethylester (2.1 g, 20 mmol), diisopropyl ethyl amine (2.6 g, 20 mmol) in THF (70 mL) was stirred at room temperature for 16 h. The reaction mixture was partitioned between saturated aqueous sodium chloride and ethyl acetate. The organic solution was separated, dried and evaporated under reduced pressure. The residue was purified using flash silica gel column chromatography using ethyl acetate/hexanes to obtain ethyl 2-(5-bromopyridine-3-sulfonamido)acetate (600 mg, 14%); LCMS Method T: retention time 1.31 min; [M+1]=323, 325.

WORKUP

后处理

  1. customThe reaction mixture was partitioned between saturated aqueous sodium chloride and ethyl acetate
  2. customThe organic solution was separated
  3. customdried
  4. customevaporated under reduced pressure
  5. customThe residue was purified