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Benzaldehyde → (1S,2S)-N-benzylcyclohexane-1,2-diamine

HRID 1528289
ノート
印刷プレビュー

反応式

HRID 1528289 の反応式
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CO.[C@H:11]1([NH2:18])[CH2:16][CH2:15][CH2:14][CH2:13][C@@H:12]1[NH2:17].[BH4-].[Na+]>O>[CH2:1]([NH:17][C@H:12]1[CH2:13][CH2:14][CH2:15][CH2:16][C@@H:11]1[NH2:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 240BenzaldehydeHCID 887MethanolHCID 4793071,2-Diaminocyclohexane, (+)-HCID 4311764Sodium borohydride

生成物 1

HCID 70610516(1S,2S)-N-benzylcyclohexane-1,2-diamine収率 48%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Benzaldehyde (3.05 mL, 30.0 mmol) was added to a methanol (300 mL) solution of (1S,2S)-cyclohexane-1,2-diamine (3.43 g, 30.0 mmol) with stirring at room temperature, and the mixture was stirred overnight at the same temperature. The reaction mixture was cooled to 0° C. Sodium borohydride (2.27 g, 60.0 mmol) was added thereto, and the mixture was stirred at 0° C. for 2 hours. To the reaction mixture, water (30 mL) was added, and the product was extracted twice with methylene chloride (50 mL). The organic layers were combined and dried over magnesium sulfate, and the solvent was then distilled off under reduced pressure. The obtained residue was purified by basic silica gel column chromatography (ethyl acetate/hexane) to obtain (1S,2S)-N-benzylcyclohexane-1,2-diamine (cas no. 207450-11-1) (2.95 g, yield: 48%) in a pale yellow oil form.

後処理

  1. stirringthe mixture was stirred overnight at the same temperature
  2. temperatureThe reaction mixture was cooled to 0° C
  3. stirringthe mixture was stirred at 0° C. for 2 hours
  4. extractionthe product was extracted twice with methylene chloride (50 mL)
  5. dry with materialdried over magnesium sulfate
  6. distillationthe solvent was then distilled off under reduced pressure
  7. customThe obtained residue was purified by basic silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-4cf198e4c3ba453d81b511f70db8e6c6
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090572B2

反応ノート

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