HRID846662

反应详情

EQUATION

反应方程式

HRID 846662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Butyl lithium (48 mL, 0.08 mol) was added at -78° C. to a stirred solution of (R)-t-butyl 2-(2,2-dibromoethenyl)-1-pyrrolidinecarboxylate (14.2 g, 0.04 mol) in dry THF (300 mL). The color turned to dark yellow. After 15 min. methanol (10 mL) and ethyl acetate (10 mL) were added and the solution was allowed to warm to room temperature. The solvent was removed and the residue was partitioned between ethyl acetate and water. The ethyl acetate phase was concentrated and applied to a silica gel column. Elution with ethyl acetate:Skellysolve B (1:10) gave 6.9 g (88%) of product as a yellow oil.

WORKUP

后处理

  1. customThe solvent was removed
  2. customthe residue was partitioned between ethyl acetate and water
  3. concentrationThe ethyl acetate phase was concentrated
  4. washElution with ethyl acetate:Skellysolve B (1:10)