HRID2209275

反应详情

EQUATION

反应方程式

HRID 2209275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Into the solution of tert-butyl 4-(6-bromopyridin-3-yl)piperazine-1-carboxylate 7.13 (1.65 g, 4.8 mmol) in THF (30 mL) was added 1M solution of n-BuLi in hexane (5 mL) and n-Bu3SnCl (1.66 g, 5.1 mmol) at −70° C. After 30 min., the reaction was warmed up to rt. After stirring for 1 h., the reaction mixture was extracted with ethyl acetate and washed with brine. After drying with MgSO4, the organic solvent was removed under vaco., the residue was purified by silica gel chromatography to obtain 0.58 g of tert-butyl 4-(6-(tributylstannyl)pyridin-3-yl)piperazine-1-carboxylate 7.14. LCMS [M+H]+: 554.07.

WORKUP

后处理

  1. extractionthe reaction mixture was extracted with ethyl acetate
  2. washwashed with brine
  3. dry with materialAfter drying with MgSO4
  4. customthe organic solvent was removed under vaco
  5. custom, the residue was purified by silica gel chromatography