Water → HCID 57486896、化合物

To a solution of 7-ethenyl-3,4-dihydro-1(2H)-isoquinolinone (224 mg, 1.295 mmol) in toluene (2 ml) and tetrahydrofuran (2 ml) at 0° C. was added sodium hydride (60% in oil, 37 mg, 1.554 mmol). The reaction mixture was warmed to room temperature and stirred for 0.5 h before addition of iodomethane (242 μl, 3.885 mmol). The reaction mixture was stirred at room temperature for 1 h before addition of additional iodomethane (242 μl, 3.885 mmol). The reaction mixture was then stirred at room temperature for a further 1 h before addition of water (20 ml). The mixture was extracted with 10% methanol/dichloromethane (3×100 ml), the organic layers were dried with magnesium sulphate and evaporated. Chromatography on silica, eluting with 0-100% ethyl acetate/hexane, gave the product (181 mg, 75%).

1. extractionThe mixture was extracted with 10% methanol/dichloromethane (3×100 ml)
2. dry with materialthe organic layers were dried with magnesium sulphate
3. customevaporated
4. washChromatography on silica, eluting with 0-100% ethyl acetate/hexane

ORDレコード

ord-ab1fa592bb99465b8b8a7b4b43aa06d2

出典データセット

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07732461B2