Hydrazine hydrate (1:1) → 4-Methoxy-3-(4-methylpiperazin-1-yl)aniline

HRID 1721311ノート

反応式

HRID 1721311 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[C:12]([N+:14]([O-])=O)[CH:11]=[CH:10][C:9]=2[O:17][CH3:18])[CH2:4][CH2:3]1.O.NN>C(O)C.[Ni].O>[CH3:18][O:17][C:9]1[CH:10]=[CH:11][C:12]([NH2:14])=[CH:13][C:8]=1[N:5]1[CH2:4][CH2:3][N:2]([CH3:1])[CH2:7][CH2:6]1

参加物

6

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 104448521-(2-Methoxy-5-nitrophenyl)-4-methylpiperazine

生成物 1

HCID 103311014-Methoxy-3-(4-methylpiperazin-1-yl)aniline収率 53%

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of the product of step (a) (5.07 g) in ethanol (70 ml) was added a paste of Raney Nickel in water (2 g). To the warmed suspension was added, with constant agitation, hydrazine hydrate (5 ml) dropwise during 20 min with occasional warming. After the main effervescence had ceased, the suspension was heated for 15 min and then filtered with the aid of ethanol under nitrogen. The residues were kept moist and washed with ethanol and the combined filtrate and washings were evaporated to dryness with the aid of ethanol. The dark residue was re-evaporated with ethanol (20 ml), resuspended in ether (40 ml) and the mixture filtered. The residue was washed with ether and dried to give a solid consisting of the title compound (2.365 g) T.l.c System A (70:8:1), Rf 0.25.

後処理

  1. temperaturethe suspension was heated for 15 min
  2. filtrationfiltered with the aid of ethanol under nitrogen
  3. washwashed with ethanol
  4. customthe combined filtrate and washings were evaporated to dryness with the aid of ethanol
  5. customThe dark residue was re-evaporated with ethanol (20 ml)
  6. filtrationthe mixture filtered
  7. washThe residue was washed with ether
  8. customdried
  9. customto give a solid

出典と根拠

ORDレコード
ord-7c59ceff150143f396a3c78dd6d750ba
出典データセット
uspto-grants-1996_04
特許番号
US05510350

反応ノート

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