HRID1721964

反应详情

EQUATION

反应方程式

HRID 1721964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

n-Butyllithium (1.5M in hexane, 12 ml) was added over 5 min to a stirred solution of 2-methyl-1,3-dithiane (2.4 g) in dry THF (30 ml) at 70° under nitrogen. The yellow solution was then stirred at -30° to -20° for 2 h, cooled to -78° and treated with a solution of the product of stage (iii) (6.1 g) in THF (25 ml). The solution was stirred at room temperature overnight, the solvent was evaporated and the residue was purified by FCC (hexane→System D 9:1) to give the title compound as a pale yellow oil (3.2 g) T.l.c. (System D 9:1) Rf 0.18.

WORKUP

后处理

  1. temperaturecooled to -78°
  2. stirringThe solution was stirred at room temperature overnight
  3. customthe solvent was evaporated
  4. customthe residue was purified by FCC (hexane→System D 9:1)