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

HRID 129157ノート

反応式

HRID 129157 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 (25g) and 25.2 g of pyridine were dissolved in 200 ml of dichloromethane to which was added dropwise 33.3 g of phenyl chloroformate with ice cooling. After stirring for 30 minutes with ice cooling, the reaction solution was washed with water and dried followed by distilling the solvent to give a mixture of phenyl 2,4-difluorophenylcarbamate and pyridine. To the mixture was added 30.7 g of 2-(di-ethoxy)ethylamine and the mixture was stirred at room temperature. The crystals separated out were filtered 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. washthe reaction solution was washed with water
  2. customdried
  3. distillationby distilling the solvent
  4. customto give
  5. stirringthe mixture was stirred at room temperature
  6. customThe crystals separated out
  7. filtrationwere filtered
  8. washwashed with petroleum ether

出典と根拠

ORDレコード
ord-458278adf92941f1a13d84297af8e95b
出典データセット
uspto-grants-1995_11
特許番号
US05466820

反応ノート

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