Ammonium Hydroxide → 6,7,8,9,10,11-Hexahydro-3-Methoxy-5-Methyl-5,10-Methano-5H-Benzocyclononen-12-Amine

HRID 1076813ノート

反応式

HRID 1076813 の反応式
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]2[CH2:7][CH:8]3[C:14](=O)[C:13]([CH3:16])([C:5]=2[CH:4]=1)[CH2:12][CH2:11][CH2:10][CH2:9]3.[OH-].[NH4+:20].[H][H]>[Ni].C(O)C>[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]2[CH2:7][CH:8]3[CH:14]([NH2:20])[C:13]([CH3:16])([C:5]=2[CH:4]=1)[CH2:12][CH2:11][CH2:10][CH2:9]3

参加物

6

反応物 3

HCID 14923Ammonium HydroxideHCID 214101236,7,8,9,10,11-hexahydro-3-methoxy-5-methyl-5,10-methano-5H-benzocyclononen 12-oneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 214100706,7,8,9,10,11-Hexahydro-3-Methoxy-5-Methyl-5,10-Methano-5H-Benzocyclononen-12-Amine

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

6,7,8,9,10,11-Hexahydro-3-methoxy-5-methyl-5,10-methano-5H-benzocyclononen-12-one, oxime (15 g. 0.058 m.) Raney nickel (3 tsps.) ethanol (100 ml.) and concentrated ammonium hydroxide (50 ml.) are shaken with hydrogen at 45 psi and 45° C. The catalyst is removed by filtration and the filtrate concentrated to remove solvent. The residue is distilled under reduced pressure to afford the title product (11 g.), b.p. 140°-142° C. (0.2 mm.) HCl salt, m.p. 298°-299° C.

後処理

  1. customThe catalyst is removed by filtration
  2. concentrationthe filtrate concentrated
  3. customto remove solvent
  4. distillationThe residue is distilled under reduced pressure

出典と根拠

ORDレコード
ord-277831e9f89141d5946d16b5c9fabf7b
出典データセット
uspto-grants-1976_05
特許番号
US03957872

反応ノート

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