HRID9093
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 stirred solution of ethyl-2-amino-4-methyl-thiazole-5-carboxylate (558 mg, 3 mmol) in dichloromethane (15 mL) and pyridine (5 mL) was treated with methanesulfonyl chloride (687 mg, 6 mmol) at rt overnight. The solution was diluted with dichloromethane (50 mL) and washed with 2N aq. HCl solution (15 mL, 3×), dried (MgSO4), filtered and concentrated. The crude residue was diluted with ether (25 mL) and the solid was filtered, washed with 1:1 ether:hexane mixture (10 mL, 3×), and dried in vacuo to obtain the title compound (687 mg, 87%) as an off-white solid.
WORKUP
后处理
- washwashed with 2N aq. HCl solution (15 mL, 3×)
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- additionThe crude residue was diluted with ether (25 mL)
- filtrationthe solid was filtered
- washwashed with 1:1 ether
- dry with materialhexane mixture (10 mL, 3×), and dried in vacuo