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
4.9 g of 4-(5-undecyl-pyrimidin-2-yl)phenol, 1.7 g of 3-propyloxy-isoxazole-5-carboxylic acid (prepared as described by Xue et al., Bioorg. Med. Chem. Letters 8 (1998) 3499 by reacting methyl 3-hydroxy-isoxazole-5-carboxylate, which is commercially available, with 1-bromopropane at 60° C. in dimethylformamide/potassium carbonate followed by hydrolysis with LiOH in tetrahydrofuran) and 2.1 g of dicyclohexylcarbodiimide are stirred for 24 h in 50 ml of dichloromethane at room temperature. Filtration, removal of the dichloromethane by distillation, purification by chromatography (silica gel; dichloromethane/heptane) and recrystallization from acetonitrile affords the target compound as colorless crystals having the phase sequence X 91 SA 109 N 126 I.
WORKUP
后处理
- filtrationFiltration, removal of the dichloromethane
- distillationby distillation, purification
- customby chromatography (silica gel; dichloromethane/heptane) and recrystallization from acetonitrile