HRID518980

反应详情

EQUATION

反应方程式

HRID 518980 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 3-(7-isopropenyl-4-methyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-ylamino)-azetidine-1-carboxylic acid tert-butyl ester (1.15 g, 2.69 mmol) and 10% Pd/C (0.2 g) in MeOH (150 mL) was stirred under H2 at 55 PSI overnight. The reaction mixture was filtered through a pad of Celite® and the filtrate was evaporated in vacuo. The residue was purified by preparative HPLC (Table 3, Method 2) to give 3-(7-isopropyl-4-methyl-3-oxo-2,3,4,10-tetrahydro-9-oxa-1,2,4a-triaza-phenanthren-6-ylamino)-azetidine-1-carboxylic acid tert-butyl ester as a white solid (0.86 g, 74%). LC/MS (Table 1, Method 2) Rt=1.186 min.; MS m/z: 452.1 [M+23]+.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through a pad of Celite®
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was purified by preparative HPLC (Table 3, Method 2)