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

HRID 223277

반응식

HRID 223277 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-158ec3ab0f664ddd8feb3e98ca716c91
출처 데이터셋
uspto-grants-1982_10
특허 번호
US04352913

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