HRID2265826
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 (510 mg, 2.3 mmol) in 29 ml tetrahydrofuran were added, at room temperature, triethylamine (0.35 ml, 2.5 mmol) and 3-(trifluoromethyl)phenyl isothiocyanate (872 μl, 5.74 mmol). The mixture was heated to reflux for 72 hours, concentrated and purified by column chromatography on silica gel (eluent: 1:2 ethyl acetate/hexane). The product was obtained in a yield of 483 mg (50%).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux for 72 hours
- concentrationconcentrated
- custompurified by column chromatography on silica gel (eluent: 1:2 ethyl acetate/hexane)
- customThe product was obtained in a yield of 483 mg (50%)