N-methylhydroxylamine hydrochloride → HCID 323917, 화합물

HRID 1578931노트

반응식

HRID 1578931 반응식
[Na].[CH3:2][C:3]([C:5]1[C:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)=[C:9]([NH2:18])[N:8]=[C:7]([NH2:19])[N:6]=1)=O.Cl.[CH3:21][NH:22][OH:23]>>[CH3:2][C:3]([C:5]1[C:10]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)=[C:9]([NH2:18])[N:8]=[C:7]([NH2:19])[N:6]=1)=[N+:22]([CH3:21])[O-:23]

참가 물질

4

반응물 3

HCID 77906N-methylhydroxylamine hydrochlorideHCID 5360545SodiumHCID 21557324HCID 21557324, 화합물

생성물 1

HCID 323917HCID 323917, 화합물

실험 절차

To a solution of sodium metal (0.6 g.) in absolute alcohol (20 ml.) was added [2,6-diamino-5-(p-chlorophenyl)-4-pyrimidinyl] methyl ketone (2.0 g.) and N-methyl hydroxylamine hydrochloride (1.2 g.), and the mixture was refluxed together for 5 hours. After removal of ethanol, the residue was filtered and recrystallized from ethanol-chloroform to give α-methyl-α-[2,6-diamino-5-(p-chlorophenyl)-4-pyrimidinyl]-N-methylnitrone as a white solid, m.p. 306°-309° (decomposition).

후처리

  1. temperaturethe mixture was refluxed together for 5 hours
  2. customAfter removal of ethanol
  3. filtrationthe residue was filtered
  4. customrecrystallized from ethanol-chloroform

출처 및 근거

ORD 기록
ord-d367dec8b13e499aa6c02f9cb6f3d415
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03940393

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