HRID9087
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 suspension of ethyl-2-amino-4-methyl-thiazole-5-carboxylate (18.6 g, 100 mmol), di-t-butyldicarbonate (26.2 g, 120 mmol) and 4-dimethylaminopyridine (800 mg, 6.55 mmol) in dry tetrahydrofuran (300 mL) was stirred under nitrogen for 18 h. The solvent was evaporated in vacuo. The residue was suspended in dichloromethane (1 L) and filtered through a pad of celite. The filtrate was washed with 1 N aqueous HCl solution (300 mL, 2×), water and brine, dried (MgSO4), and concentrated in vacuo. The residue was triturated with hexanes. The solid was filtered and dried in vacuo to obtain the title compound (20 g, 72%) as a tan solid.
WORKUP
后处理
- customThe solvent was evaporated in vacuo
- filtrationfiltered through a pad of celite
- washThe filtrate was washed with 1 N aqueous HCl solution (300 mL, 2×), water and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was triturated with hexanes
- filtrationThe solid was filtered
- customdried in vacuo