HRID635845
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was heated
- temperatureto reflux temperature for 22 hours
- temperatureThe reaction was cooled to 25°
- customthe solvent evaporated to an orange oil (17 g)
- customThe oil was triturated with hexane
- customto yield yellow crystals
- customRecrystallization
- temperaturefrom warm hexane