Chloroform → 1-(2-Cyanoethylamino)-5-(4,6-dimethyl-2-pyrimidylamino)pentane

HRID 34753

反応式

HRID 34753 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([NH:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][NH2:15])[N:3]=1.[C:16](#[N:19])[CH:17]=[CH2:18].C(Cl)(Cl)Cl>C(O)(C)(C)C>[C:16]([CH2:17][CH2:18][NH:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][NH:9][C:4]1[N:5]=[C:6]([CH3:8])[CH:7]=[C:2]([CH3:1])[N:3]=1)#[N:19]

参加物

5

反応物 3

HCID 6212ChloroformHCID 7855AcrylonitrileHCID 143460175-(4,6-Dimethyl-2-pyrimidylamino)-1-pentanamine

生成物 1

HCID 143460181-(2-Cyanoethylamino)-5-(4,6-dimethyl-2-pyrimidylamino)pentane収率 85.8%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒2 回

実験手順

To a stirred solution of (XII) (966 mg) in t-butanol was added 250 mg of acrylonitrile dissolved in 1 ml t-butanol over a period of 1 hour. Continued stirring for 3.5 hours at room temperature and finally refluxed for 1.5 hours. Chloroform was added and the product was extracted into 1N H2SO4. The aqueous phase was washed once with CHCl3, then basified to pH 10 with 2N NaOH and the free amine extracted into CHCl3. The product (XIII) 1.04 g was obtained by evaporation of the solvents under vacuum.

後処理

  1. temperaturefinally refluxed for 1.5 hours
  2. extractionthe product was extracted into 1N H2SO4
  3. washThe aqueous phase was washed once with CHCl3
  4. extractionthe free amine extracted into CHCl3

出典と根拠

ORDレコード
ord-910574ed73dc41d5b4fcb1ab0f5d4a28
出典データセット
uspto-grants-1988_08
特許番号
US04762949

関連ノート

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