HRID494139

反应详情

EQUATION

反应方程式

HRID 494139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (6S)-4-amino-2-(3-chloro-4-fluorobenzyl)-10-methoxy-8-ethyl-6-methyl-7,8-dihydropyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione (62 mg, 0.14 mmol) in anhydrous dichloromethane (2 mL), a solution of boron tribromide in dichloromethane (0.43 mL, 0.43 mmol; 1 M) was added. After stirring at room temperature for 30 minutes, the reaction mixture was treated with anhydrous methanol, stirred for 30 minutes, and concentrated under vacuum. The procedure was repeated twice. The residue was subjected to purification on preparative reverse phase high pressure column chromatography. Collection and lyophilization of appropriate fractions provided the title compound.

WORKUP

后处理

  1. stirringstirred for 30 minutes
  2. concentrationconcentrated under vacuum
  3. customThe residue was subjected to purification on preparative reverse phase high pressure column chromatography
  4. customCollection and lyophilization of appropriate fractions