Ammonia → 4-(3-Aminopropyl)-4-cyclohexylpiperidine-1-carboxylic acid tert-butyl ester

HRID 1795175ノート

反応式

HRID 1795175 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([CH:20]=[CH:21][C:22]#[N:23])([CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].N>CO.[Ni]>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][C:11]([CH2:20][CH2:21][CH2:22][NH2:23])([CH:14]2[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19]2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 2

HCID 222AmmoniaHCID 695970864-(2-Cyanovinyl)-4-cyclohexylpiperidine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 210237744-(3-Aminopropyl)-4-cyclohexylpiperidine-1-carboxylic acid tert-butyl ester

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

To a solution of 4-(2-cyanovinyl)-4-cyclohexylpiperidine-1-carboxylic acid tert-butyl ester, 14, (800 mg, 2.35 mmol) in MeOH (33 mL) is added ammonia (16 mL) and Raney Ni (50 mg). The reaction mixture is degassed with nitrogen, purged with hydrogen gas and shaken under an atmosphere of hydrogen (45 psi) on a standard hydrogenation apparatus at room temperature for 6 hours. The reaction solution is filtered to remove the catalyst and the solvent removed in vacuo to afford the desired product was obtained as a colorless, sticky oil in quantitative yield.

後処理

  1. customThe reaction mixture is degassed with nitrogen
  2. custompurged with hydrogen gas
  3. filtrationThe reaction solution is filtered
  4. customto remove the catalyst
  5. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-6d37f3a415b64af89315f71cd3701724
出典データセット
uspto-grants-2006_04
特許番号
US07026335B2

反応ノート

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