Water → Hexahydrofuro[2,3-b]furan-3-yl acetate

温度

2.5 °C

Hexahydrofuro[2,3-b]furan-3-ol (IV, 60 g) was dissolved in dichloromethane (300 mL) and cooled to 0-5° C. To the cooled solution triethylamine (58.2 g), N,N-dimethylaminopyridine (1.12 g) was added, acetic anhydride (56.5 g) was added for 30-60 minutes at the same temperature, the mass temperature was raised to 25-35° C. and stirred for 2-4 hours. After completion of reaction the mass was cooled to 10-20° C., water (120 mL) was added, stirred for 30 minutes, separated the organic layer, washed with 10% sodium chloride solution (120 mL) and distilled out dichloromethane to get title compound (yield 72 g). Further, the product was purified by fractional distillation to get pure Hexahydrofuro[2,3-b]furan-3-yl acetate III (yield 54 g).

1. temperaturethe mass temperature was raised to 25-35° C.
2. customAfter completion of reaction the mass
3. temperaturewas cooled to 10-20° C.
4. stirringstirred for 30 minutes
5. customseparated the organic layer
6. washwashed with 10% sodium chloride solution (120 mL)
7. distillationdistilled out dichloromethane

ORDレコード

ord-cca1ab0112f444b48d561ee32f866e66

出典データセット

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09216990B2