Hydrazine hydrate (1:1) → 3-Benzyl-3-azabicyclo(3.1.0)hexan-6-amine

HRID 712482ノート

反応式

HRID 712482 の反応式
[CH2:1]([N:8]1[CH2:13][CH:12]2[CH:10]([CH:11]2[N+:14]([O-])=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.NN.O>[Ni].CO>[CH2:1]([N:8]1[CH2:13][CH:12]2[CH:10]([CH:11]2[NH2:14])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 215851823-Benzyl-6-nitro-3-azabicyclo[3.1.0]hexane

生成物 1

HCID 185069973-Benzyl-3-azabicyclo(3.1.0)hexan-6-amine収率 104.3%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

To a mixture of 3-benzyl-6-nitro-3-azabicyclo[3.1.0]hexane (4.00 g) and a catalytic amount of Raney nickel in MeOH was added slowly a solution of 98% H2NNH2—H2O (70 mL) at rt. The mixture was stirred for 5 h at room temperature and filtered. The filtrate was concentrated in vacuo to give the title compound as brown oil (3.60 g) and the crude product was used for the next step without further purification. The compound was characterized by the following spectroscopic data: MS (ESI, pos. ion) m/z: 204.3 (M+1).

後処理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-a3338bfb92f0451ca9e679207868fa8a
出典データセット
uspto-grants-2015_11
特許番号
US09181277B2

反応ノート

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