Pyridine → 2-[2-(1-Azabicyclo[3.3.0]octan-5-yl)ethylamino]benzonitrile

HRID 260928ノート

反応式

HRID 260928 の反応式
F[C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[N:10]12[CH2:17][CH2:16][CH2:15][C:14]1([CH2:18][CH2:19][NH2:20])[CH2:13][CH2:12][CH2:11]2.N1C=CC=CC=1>O>[N:10]12[CH2:17][CH2:16][CH2:15][C:14]1([CH2:18][CH2:19][NH:20][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5])[CH2:13][CH2:12][CH2:11]2

参加物

5

反応物 3

HCID 1049PyridineHCID 678552-FluorobenzonitrileHCID 107969772-(Hexahydro-1H-pyrrolizin-7a-yl)ethanamine

生成物 1

HCID 107535222-[2-(1-Azabicyclo[3.3.0]octan-5-yl)ethylamino]benzonitrile収率 95.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Fluorobenzonitrile (1.00 g, 8.26 mmol) and 2-(1-azabicyclo[3.3.0]octan-5-yl)ethylamine (3.15 g, 20.4 mmol) were added into anhydrous pyridine (10.0 ml) to react the mixture in a sealed tube for 10.5 hours at 180° C. After addition of water subsequent to concentration in vacuo, the reaction mixture was extracted by ethyl acetate, dried over anhydrous sodium sulfate, concentrated in vacuo, and refined by column chromatography to afford the desired compound (2.02 g, 95.8%), as a colorless liquid.

後処理

  1. customto react the mixture in a sealed tube for 10.5 hours at 180° C
  2. concentrationto concentration in vacuo
  3. extractionthe reaction mixture was extracted by ethyl acetate
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-fc2793cb99ee48efbbc4e595b548bf94
出典データセット
uspto-grants-1996_06
特許番号
US05530138

反応ノート

読み込み中…