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

HRID 1112570ノート

反応式

HRID 1112570 の反応式
[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

参加物

4

反応物 2

HCID 14232N,O-DimethylhydroxylamineHCID 22762251HCID 22762251、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3cb20502903140ee8aefd57c2f780501
出典データセット
uspto-grants-1978_10
特許番号
US04123256

反応ノート

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