Pyridine → N-(2,2-diethoxyethyl)-N'-(2,4-difluorophenyl)urea

HRID 482044ノート

反応式

HRID 482044 の反応式
[F:1][C:2]1[CH:8]=[C:7]([F:9])[CH:6]=[CH:5][C:3]=1[NH2:4].N1C=CC=[CH:12][CH:11]=1.Cl[C:17]([O:19][C:20]1[CH:25]=CC=CC=1)=[O:18].FC1C=C(F)C=C[C:28]=1[NH:34][C:35](=O)[O:36]C1C=CC=CC=1>ClCCl>[CH2:20]([O:19][CH:17]([O:18][CH2:11][CH3:12])[CH2:28][NH:34][C:35]([NH:4][C:3]1[CH:5]=[CH:6][C:7]([F:9])=[CH:8][C:2]=1[F:1])=[O:36])[CH3:25]

参加物

6

反応物 4

HCID 1049Pyridine2 回HCID 97092,4-DifluoroanilineHCID 15891Phenyl chloroformateHCID 13733129phenyl N-(2,4-difluorophenyl)carbamate

生成物 1

HCID 19065111N-(2,2-diethoxyethyl)-N'-(2,4-difluorophenyl)urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2,4-Difluoroaniline (25 g) and 25.2 g of pyridine were dissolved in 200 ml of dichloromethane and, with ice cooling, 33.3 g of phenyl chloroformate was added dropwise thereinto. The reaction solution was stirred with ice cooling for 30 minutes, washed with water and dried. The solvent was distilled off to give a mixture of phenyl 2,4-difluorophenylcarbamate and pyridine. To the mixture was added 30.7 g of 2-(diethoxy)ethylamine, and the resulting mixture was stirred at room temperature. The crystals separated out were collected by filtration and washed with petroleum ether to give 37.8 g of N-(2,2-diethoxyethyl)-N'-(2,4-difluorophenyl)urea as colorless crystals.

後処理

  1. additionwas added dropwise
  2. washwashed with water
  3. customdried
  4. distillationThe solvent was distilled off
  5. customto give
  6. stirringthe resulting mixture was stirred at room temperature
  7. customThe crystals separated out
  8. filtrationwere collected by filtration
  9. washwashed with petroleum ether

出典と根拠

ORDレコード
ord-648134d0e1e04ea7aec0bf4feb4a5a2f
出典データセット
uspto-grants-1998_08
特許番号
US05792780

反応ノート

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