HRID2265822
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 4,4-bis(hydroxymethyl)-3,4-dihydro-2H-benzo[b]thiepin-5-one (476 mg, 2.0 mmol) in 15 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.31 ml, 2.2 mmol) and 1-naphthyl isothiocyanate (407 mg, 2.2 mmol). The mixture was heated to reflux for 24 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:19 tert-butyl methyl ether/dichloromethane). The product was obtained in a yield of 87 mg (9%).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 24 hours
- concentrationconcentrated
- custompurified by column chromatography on silica gel (eluent: 1:19 tert-butyl methyl ether/dichloromethane)
- customThe product was obtained in a yield of 87 mg (9%)