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

HRID 1491781노트

반응식

HRID 1491781 반응식
[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]

참가 물질

6

반응물 4

HCID 1049Pyridine2회HCID 97092,4-DifluoroanilineHCID 15891Phenyl chloroformateHCID 13733129phenyl N-(2,4-difluorophenyl)carbamate

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-27d3d361b5c9457d8b55321fad014469
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05371101

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