Potassium Hydroxide → 4-Aminostyrene

温度

240 °C

A mixture of 2-(4-aminophenyl)ethanol (10 g, 73 mmol), KOH (25 g, 450 mmol) and t butylcatechol (0.1 g) was heated at 240° C./40 mmHg in a flask fitted with a water-cooled condenser for 90 minutes. The contents of the flask were then distilled into a receiver vessel as a clear, 2-phase system which sodified as white crystals on standing. The solid was extracted with 50 ml diethyl ether, washed twice with 25 ml distilled water and the organic phase separated. After drying for 2 hours over NaOH pellets, the ether solution was filtered and the volatiles removed in vacuo to yield a colourless crystalline solid. Fractional distillation at 38° C. (1×10-2 mbar) yielded 4-aminostyrene. The colourless liquid was stored at -30° C. (at which temperature it is a crystalline solid) to prevent polymerisation.

1. temperaturecooled condenser for 90 minutes
2. distillationThe contents of the flask were then distilled into a receiver vessel as a clear, 2-phase system which
3. extractionThe solid was extracted with 50 ml diethyl ether
4. washwashed twice with 25 ml
5. distillationdistilled water
6. customthe organic phase separated
7. dry with materialAfter drying for 2 hours over NaOH pellets
8. filtrationthe ether solution was filtered
9. customthe volatiles removed in vacuo
10. customto yield a colourless crystalline solid
11. distillationFractional distillation at 38° C. (1×10-2 mbar)

ORDレコード

ord-91fbfbe7701a4a13bfb8be8af184cc24

出典データセット

uspto-grants-2000_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06015767