N,N-Dimethyl-1,3-propanediamine → Urea, N,N''-1,6-hexanediylbis[N'-[3-(dimethylamino)propyl]-

HRID 223277

反応式

HRID 223277 の反応式
[CH3:1][N:2]([CH2:4][CH2:5][CH2:6][NH2:7])[CH3:3].[CH2:8]([N:17]=[C:18]=[O:19])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][N:14]=[C:15]=[O:16]>C(Cl)Cl>[N:2]([CH2:4][CH2:5][CH2:6][NH:7][C:15]([NH:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][NH:17][C:18]([NH:7][CH2:6][CH2:5][CH2:4][N:2]([CH3:3])[CH3:1])=[O:19])=[O:16])([CH3:3])[CH3:1]

参加物

4

反応物 2

HCID 7993N,N-Dimethyl-1,3-propanediamineHCID 13192Hexamethylene diisocyanate

生成物 1

HCID 335058Urea, N,N''-1,6-hexanediylbis[N'-[3-(dimethylamino)propyl]-収率 59.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

204.3 g of dimethylaminopropylamine are added dropwise to a solution of 168.2 g of hexamethylene diisocyanate in 100 ml of methylene chloride and the mixture is refluxed overnight, in the process of which crystals precipitate. The crystals are filtered with suction at room temperature, washed with CH2Cl2 and dried. Recrystallisation from a mixture of 1000 ml of acetone and 800 ml of ethanol yields 221.0 g (59.3%) of product with a melting point of 159° C. Tritration: 2 equivalents=376.7 g (theory 372.6 g).

後処理

  1. temperaturethe mixture is refluxed overnight, in the process of which crystals
  2. customprecipitate
  3. filtrationThe crystals are filtered with suction at room temperature
  4. washwashed with CH2Cl2
  5. customdried
  6. customRecrystallisation
  7. additionfrom a mixture of 1000 ml of acetone and 800 ml of ethanol

出典と根拠

ORDレコード
ord-158ec3ab0f664ddd8feb3e98ca716c91
出典データセット
uspto-grants-1982_10
特許番号
US04352913

関連ノート

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