HRID2419325
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 of 4-acetamido-2-bromothiazole and methyl tosylate (4.65 g, 25 mM) in dry acetonitrile (125 ml) was treated with a 60% dispersion of sodium hydride in oil (1 g, 25 mM) and the mixture stirred 72 hours at ambient temperature. The reaction mixture was filtered and the filtrate evaporated under reduced pressure. The residue was chromatographed on silica (Woelm grade 1, 150 g) using 2% methanol in chloroform as eluant. Evaporations of the appropriate fractions followed by recrystallisation from hexane gave 2-bromo-4-(N-methylacetamido)thiazole (1.9 g, 32%) mp 84° C. Found: C, 30.55; H, 2.95; N, 11.8%, C6H7N2BrOS requires C, 30.7; H, 3.0; N, 11.9%).
WORKUP
后处理
- filtrationThe reaction mixture was filtered
- customthe filtrate evaporated under reduced pressure
- customThe residue was chromatographed on silica (Woelm grade 1, 150 g)
- customEvaporations of the appropriate fractions followed by recrystallisation from hexane