反応 #63139

ord-84e111d02c504196864cc1b3e0ea59c4

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture is then heated to the reflux temperture for 12 hours
  2. 2
    workup.DISTILLATIONThereafter, 90% of the pyridine is distilled off
  3. 3
    ろ過The crystalline product is filtered off under suction
  4. 4
    洗浄washed with a little water
  5. 5
    その他dried

実験手順

100 g of 2,3,4-trichlorobenzotrifluoride are initially introduced, 200 ml of pyridine are added, followed by 100 g of hydrazine hydrate and the mixture is then heated to the reflux temperture for 12 hours. Thereafter, 90% of the pyridine is distilled off and the remaining residue is stirred into 250 ml of water. The crystalline product is filtered off under suction, washed with a little water and dried. 78 g of 2,3-dichloro-4-trifluoromethyl-phenylhydrazine having a melting point of 79° to 80° C. are obtained.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04764202uspto-grants-1988_08