HRID2237386

反应详情

EQUATION

反应方程式

HRID 2237386 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of 5-bromo-1,2,3,4-tetrahydro-2-methylisoquinolin-8-amine (IV, 3.25 g, 13.5 mmol), chloral hydrate (2.3 g), hydroxylamine hydrochloride (2.9 g), 12 g Na2SO4 (12 g) in H2O:EtOH (3:1, 50 mL) was refluxed for 1 hr whereafter it was cooled to 60° C. and carefully basified with 4N NaOH to pH=7 and allowed to cool. The solid was collected by filtration, washed with water and dried under vacuum to give V.

WORKUP

后处理

  1. temperaturewas refluxed for 1 hr whereafter it
  2. temperatureto cool
  3. filtrationThe solid was collected by filtration
  4. washwashed with water
  5. customdried under vacuum
  6. customto give V