HRID2223434
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
2-tetradecylthioacetamidopropan-1,3-diol (1 g, 2.77 mmol) (example 5a) was dissolved in dichloromethane (180 ml), then dicyclohexycarbodiimide (1.427 g, 6.91 mmol), dimethylaminopyridine (0.845 g, 6.91 mmol) and tetradecylthioacetic acid (1.995 g, 6.91 mmol) (example 1a) were added in that order. The reaction mixture was stirred at room temperature for 48 hours. The dicyclohexylurea precipitate was filtered and washed with dichloromethane and the filtrate was concentrated. The residue obtained was purified by silica gel chromatography (eluent:dichloromethane-cyclohexane 7:3). The desired compound was obtained as a white powder (yield: 66%).
WORKUP
后处理
- additionwere added in that order
- filtrationThe dicyclohexylurea precipitate was filtered
- washwashed with dichloromethane
- concentrationthe filtrate was concentrated
- customThe residue obtained
- customwas purified by silica gel chromatography (eluent:dichloromethane-cyclohexane 7:3)