5-Fluorosalicylaldoxime → 5-Fluoro-2-hydroxybenzonitrile

温度

80 °C

5-Fluorosalicylaldehyde oxime (20.2 g, 0.13 mol) was dissolved in acetic anhydride (100 ml) and refluxed for 5 hours. After completion of the reaction, acetic anhydride was distilled off under reduced pressure, followed by adding to the remaining oily substance, a solution of KOH (20 g) dissolved in water (100 ml) and ethanol (100 ml), warming the mixture at 80° C. for 2 hours, allowing it to cool down to room temperature, adding 6N hydrochloric acid (50 ml) and water (200 ml) to deposit crystals, which were then filtered off and recrystallized from methanol (30 ml) to obtain needle crystals (15.6 g) having a melting point of 121°-122° C.

1. temperaturerefluxed for 5 hours
2. distillationwas distilled off under reduced pressure
3. additionby adding to the remaining oily substance
4. dissolutiona solution of KOH (20 g) dissolved in water (100 ml)
5. temperatureto cool down to room temperature
6. additionadding 6N hydrochloric acid (50 ml) and water (200 ml)
7. filtrationwere then filtered off
8. customrecrystallized from methanol (30 ml)

ORDレコード

ord-b1af9970c42a4537a7ca4b0fe2d9bb6d

出典データセット

uspto-grants-1986_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04603018