HRID255102
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
To a solution of 4,5-dimethyl-thiazol-2-ylamine hydrochloride (1.65 g, 10.0 mmol) in THF (100 mL) was added triethylamine (4.2 mL, 30 mmol) and adamantane-1-carbonyl chloride (2.2 g, 11 mmol). The mixture was heated at reflux overnight and then concentrated under reduced pressure. The residue was diluted with ethyl acetate, washed with 1M NaHCO3, dried (Na2SO4), filtered and concentrated. Purification by column chromatography (SiO2, 10% ethyl acetate:90% hexanes) afforded 2.15 g (74%) of the title compound. MS (ESI+) m/z 291 (M+H)+.
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureat reflux overnight
- concentrationconcentrated under reduced pressure
- additionThe residue was diluted with ethyl acetate
- washwashed with 1M NaHCO3
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customPurification by column chromatography (SiO2, 10% ethyl acetate:90% hexanes)