Furan → 2,5-Di-tert-butylfuran

温度

40 °C

Dichloromethane (1275 g), iron (III) oxide (200 g) and iron (III) cloride (5.0 g) were charged to a reaction vessel and the stirred mixture was heated to reflux temperature (ca. 40° C.). A mixture of furan (85.1 g) and tert.butyl chloride (289.3 g) was then run into the solvent/catalyst mixture during about 1.5 hours, and the mixture was then maintained at reflux temperature, with stirring, for a further 1.5 hours after the addition was complete. The reaction mixture was then filtered to remove the catalyst, which was washed on the filter with dichloromethane (2×100 g). The filtrate and washings were combined and the dichloromethane was distilled off until the internal temperature of the mixture reached 60°-65° C. Glycerol (125 g) was then added and the mixture was subjected to distillation under reduced pressure to give 2,5-di-tert.butylfuran (80 g at 85.9% strength=32% of theoretical based on furan charged) b.p. 85° C./15 mm Hg pressure (20 mbar).

1. temperaturethe stirred mixture was heated
2. temperaturethe mixture was then maintained
3. temperatureat reflux temperature
4. additionafter the addition
5. filtrationThe reaction mixture was then filtered
6. customto remove the catalyst, which
7. washwas washed on the
8. filtrationfilter with dichloromethane (2×100 g)
9. distillationthe dichloromethane was distilled off until the internal temperature of the mixture
10. customreached 60°-65° C
11. additionGlycerol (125 g) was then added
12. distillationthe mixture was subjected to distillation under reduced pressure

ORDレコード

ord-e2db6849f4734ddca4309a5ae38c19a9

出典データセット

uspto-grants-1982_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04323509