HRID2409899

反应详情

EQUATION

反应方程式

HRID 2409899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of bromo-phenyl-acetaldehyde (1 g, 5 mmol), thiourea (0.64 g, 10 mmol) and ethanol (3.5 mL) was heated to reflux overnight. The mixture was then cooled to rt and the resulting yellow precipitate filtered. The precipitate was then washed with aqueous NaHCO3 solution (10 mL) and dried. Recrystallization from 30% methanol gave 5-phenylthiazol-2-amine (500 mg, 2.84 mmol, 56.5%) as a yellow solid. Anal. Calcd. for C9H8N2S m/z 176.2, found: 177.2 (M+H)+; 1H NMR (400 MHz, DMSO-d6) δ ppm 7.41 (m, 3H), 7.33 (m, 2H), 7.18 (m, 1H), 7.13 (m, 2H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux overnight
  3. filtrationthe resulting yellow precipitate filtered
  4. washThe precipitate was then washed with aqueous NaHCO3 solution (10 mL)
  5. customdried
  6. customRecrystallization from 30% methanol