HRID2221089

反应详情

EQUATION

反应方程式

HRID 2221089 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 1E (560 mg, 1.11 mmol) and 5% wt. platinium on activated carbon (500 mg) in THF (90 mL) and MeOH (90 mL) was stirred at RT under H2 at 80 psi for 2 days. After this time, no starting material was detected by LC-MS. The reaction mixture was filtered and the filtrate was concentrated. The residue was purified by silica gel (40 g) column chromatography eluting with a gradient of EtOAc (0-60%) in hexane to give the title compound as a foam (420 mg, 75%). LC/MS (method A): retention time=3.24 min, (M+H)+=506.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by silica gel (40 g) column chromatography
  4. washeluting with a gradient of EtOAc (0-60%) in hexane