HRID635845

反应详情

EQUATION

反应方程式

HRID 635845 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution 2-amino-4-methylthiazole (Formula C-1)(11.4 g) in toluene (100 ml) at 25° was treated with dimethylformamide dimethyl acetal (15.9 mL, 200 mmol), dropwise over five minutes. The mixture was heated to reflux temperature for 22 hours. The reaction was cooled to 25° and the solvent evaporated to an orange oil (17 g). The oil was triturated with hexane to yield yellow crystals. Recrystallization from warm hexane gave N′-(4-Methyl-2-thiazolyl)-N,N-dimethyl-methanimidamide (Formula C-2) (16.9 g, 99.6%), m.p. 54-56°.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux temperature for 22 hours
  3. temperatureThe reaction was cooled to 25°
  4. customthe solvent evaporated to an orange oil (17 g)
  5. customThe oil was triturated with hexane
  6. customto yield yellow crystals
  7. customRecrystallization
  8. temperaturefrom warm hexane