反応 #4470

ord-3b691c0f3b274492971e450bdceebda6

反応方程式

O=C1CCCC(=O)C1
cyclohexane-1,3-dione
Cl.NNc1ccc(F)cc1
4-fluorophenylhydrazine hydrochloride
[Na+].[OH-]
sodium hydroxide
OC1=CC(=NNc2ccc(F)cc2)CCC1
title compound
収率 96.4%
OC1=CC(=NNc2ccc(F)cc2)CCC1
3-Hydroxy-2-cyclohexen-1-one (4-fluorophenyl)hydrazone
収率 96.4%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過the precipitate was filtered off
  2. 2
    洗浄washed with water (50 ml), air
  3. 3
    その他dried for 1 h
  4. 4
    乾燥dried in vacuo over phosphorus pentoxide at 75°

実験手順

A suspension of 4-fluorophenylhydrazine hydrochloride (50 g) in water (500 ml) was treated with sodium hydroxide (12.3 g) in water (50 ml) and the resultant solution added to solution of cyclohexane-1,3-dione (97%, 35.6 g) in water (300 ml) over 2 h under nitrogen with stirring. After a further 30 min, the precipitate was filtered off, washed with water (50 ml), air dried for 1 h, and dried in vacuo over phosphorus pentoxide at 75° to give the title compound as a powder (65.3 g) m.p. 175°-176°.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04725615uspto-grants-1988_02