HRID338724

反应详情

EQUATION

反应方程式

HRID 338724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of tert-butyl 3-oxopyrrolidine-1-carboxylate (25.0 g, 135 mmol), dimethylformamide dimethylacetal (27 mL, 202 mmol) and 1,4-dioxane (170 mL) was heated at 100° C. for 17 hours. The dioxane was removed in vacuo. The resulting red solid was triturated with hexanes (180 mL) for one hour, and filtered. The solid was rinsed with hexanes (2×80 mL) and air dried. Chromatography on silica gel eluting with dichloromethane:methanol 39:1 then 19:1 to give the title compound (15.04 g, 46%).

WORKUP

后处理

  1. customThe dioxane was removed in vacuo
  2. customThe resulting red solid was triturated with hexanes (180 mL) for one hour
  3. filtrationfiltered
  4. washThe solid was rinsed with hexanes (2×80 mL) and air
  5. customdried