HRID529526

反应详情

EQUATION

反应方程式

HRID 529526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A solution of tert-butyl (S)-1-oxo-1-((R)-2-vinylpiperidin-1-yl)pent-4-en-2-ylcarbamate (1.00 gm, 3.24 mmol) in DCE (350 mL) was purged with argon for 10 min. Grubbs II catalyst (0.124 gm, 0.146 mmol) was added and the reaction mixture was heated at 60° C. under argon for 18 hr. The reaction mixture was concentrated. The crude product was purified using silica gel chromatography (ISCO system) eluting with a gradient of 0-100% EtOAc/Hex to give tert-butyl (7S,10aR,Z)-6-oxo-1,2,3,4,6,7,8,10a-octahydropyrido[1,2-a]azepin-7-ylcarbamate (653 mg, 2.33 mmol, 71.8% yield) as a solid. Anal. Calcd. for C15H24N2O3 m/z 280.3. found: 281.0 (M+H)+.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. customThe crude product was purified
  3. washeluting with a gradient of 0-100% EtOAc/Hex