HRID2265824
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]oxepin-5-one (500 mg, 2.25 mmol) in 28 ml of tetrahydrofuran were added, at room temperature, triethylamine (0.34 ml, 2.5 mmol) and phenyl isothiocyanate (672 μl, 5.63 mmol). The mixture was heated to reflux for 72 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:1 tert-butyl methyl ether/cyclohexane). The product was obtained in a yield of 149 mg (19%).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 72 hours
- concentrationconcentrated
- custompurified by column chromatography on silica gel (eluent: 1:1 tert-butyl methyl ether/cyclohexane)
- customThe product was obtained in a yield of 149 mg (19%)