N,O-Dimethylhydroxylamine → N'-{4-[(2-Fluorophenyl)methoxy]phenyl}-N-methoxy-N-methylurea

HRID 1112570노트

반응식

HRID 1112570 반응식
[F:1][C:2]1[CH:18]=[CH:17][CH:16]=[CH:15][C:3]=1[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([N:12]=[C:13]=[O:14])=[CH:8][CH:7]=1.[CH3:19][NH:20][O:21][CH3:22]>C1C=CC=CC=1>[F:1][C:2]1[CH:18]=[CH:17][CH:16]=[CH:15][C:3]=1[CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([NH:12][C:13]([N:20]([CH3:19])[O:21][CH3:22])=[O:14])=[CH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 14232N,O-DimethylhydroxylamineHCID 22762251HCID 22762251, 화합물

생성물 1

HCID 12893493N'-{4-[(2-Fluorophenyl)methoxy]phenyl}-N-methoxy-N-methylurea수율 59.2%

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a solution of 4-(2-fluorobenzyloxy)phenyl isocyanate (24.3 g) in benzene (150 ml), a solution of N,O-dimethylhydroxylamine (20 g) in benzene (100 ml) is added dropwise at 20° to 30° C., and the resulting mixture is stirred at the same temperature for 30 minutes. The reaction mixture is concentrated in vacuo, and the residual crude crystals are recrystallized from ethanol to give N-[4-(2-fluorobenzyloxy)phenyl]-N'-methyl-N'-methoxyurea (Compound No. 1) (18 g) as white scales. M.P., 99° to 100° C.

후처리

  1. concentrationThe reaction mixture is concentrated in vacuo
  2. customthe residual crude crystals are recrystallized from ethanol

출처 및 근거

ORD 기록
ord-3cb20502903140ee8aefd57c2f780501
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04123256

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