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Hydrazine hydrate (1:1) → HCID 76568135、化合物

HRID 1728191
ノート
印刷プレビュー

反応式

HRID 1728191 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]2[NH:8][C:9](=[O:30])[C:10]3([CH:15]([C:16]4[CH:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:17]=4[N+:23]([O-])=O)[CH2:14][C:13](=[O:26])[NH:12][CH:11]3[C:27]([CH3:29])=[CH2:28])[C:5]2=[CH:4][CH:3]=1.NN.O>CO.[Ni]>[NH2:23][C:17]1[CH:18]=[CH:19][C:20]([Cl:22])=[CH:21][C:16]=1[CH:15]1[CH2:14][C:13](=[O:26])[NH:12][CH:11]([C:27]([CH3:29])=[CH2:28])[C:10]21[C:5]1[C:6](=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1)[NH:8][C:9]2=[O:30]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 76567907HCID 76567907、化合物

生成物 1

HCID 76568135HCID 76568135、化合物収率 96.1%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

The reaction mixture of racemic (2′R,3R,4′S)-6-chloro-4′-(5-chloro-2-nitro-phenyl)-2′-isopropenylspiro[3H-indole-3,3′-piperidine]-2,6′(1H)-dione (290 mg, 0.65 mmol), Raney Ni (39 mg) and NH2NH2.H2O (320 mg) in methanol was stirred at 80° C. for 0.5 h. The mixture was cooled to 4° C., and concentrated. To the residue were added ethyl acetate (10 mL) and water (10 mL). The organic layer was separated, washed with brine, dried over MgSO4 and concentrated. The residue was purified by column chromatography to give the title compound as a solid (Yield: 260 mg).

後処理

  1. temperatureThe mixture was cooled to 4° C.
  2. concentrationconcentrated
  3. additionTo the residue were added ethyl acetate (10 mL) and water (10 mL)
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated
  8. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-6e422cb4566f4f5f9a8b60d7325f69d6
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07495007B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート