4-Bromopyridine → 1-pyridin-4-yl-1,4-diazepane

HRID 1243329ノート

反応式

HRID 1243329 の反応式
Br[C:2]1[CH:7]=[CH:6][N:5]=[CH:4][CH:3]=1.[NH:8]1[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.[OH-].[Na+]>O>[N:5]1[CH:6]=[CH:7][C:2]([N:8]2[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:3][CH:4]=1

参加物

5

反応物 3

HCID 142684-BromopyridineHCID 14798Sodium HydroxideHCID 68163Hexahydro-1,4-diazepine

生成物 1

HCID 27605081-pyridin-4-yl-1,4-diazepane収率 40.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2 g of 4-bromopyridine and 10 g of homopiperazine is heated at 100° C. for 4 hours. 100 ml of water are added to the reaction mixture and the resulting mixture is basified to pH 10 by addition of 10% NaOH solution and extracted three times with 100 ml of chloroform, the organic phase is dried over Na2SO4 and the solvent is evaporated off under vacuum. 0.9 g of the expected product is obtained.

後処理

  1. extractionextracted three times with 100 ml of chloroform
  2. dry with materialthe organic phase is dried over Na2SO4
  3. customthe solvent is evaporated off under vacuum

出典と根拠

ORDレコード
ord-e45bd25b6bab40cb95ed25343601ba20
出典データセット
uspto-grants-2006_10
特許番号
US07119086B2

反応ノート

読み込み中…