HRID1161231

反应详情

EQUATION

反应方程式

HRID 1161231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(R)-3-Methyl-2-(5-nitro-1-oxoisoquinolin-2(1H)-yl)butanoic acid (2 g, 0.007 mol), methylamine (7 mL, 0.01 mol), 1-hydroxybenzotriazole hydrate (2 g, 0.01 mol), N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (3 g, 0.01 mol), N,N-diisopropylethylamine (4 g, 0.03 mol) were stirred in methylene chloride (20 mL, 0.3 mol) at room temperature for 16 hours. The reaction mixture was diluted with CH2Cl2 (200 mL), washed with sat. NaHCO3, dried over MgSO4, filtered, purified via flash chromatoraphy (40 g of silica gel, 0-50% EtOAc/Hexane) to yield a yellow solid. m/z 304.2 (M+H)+.

WORKUP

后处理

  1. washwashed with sat. NaHCO3
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. custompurified via flash chromatoraphy (40 g of silica gel, 0-50% EtOAc/Hexane)
  5. customto yield a yellow solid