2,2'-Azobis(2-methylpropanimidamide) dihydrochloride → 1,10-bis(diallylmethylammonio)decane Dibromide Diallylmethyldodecylammonium Bromide

HRID 397223

반응식

HRID 397223 반응식
[Br-:1].[Br-].[CH2:3]([CH:6]([NH2+:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH2+:21][CH:22]([CH2:26][CH:27]=[CH2:28])[CH2:23][CH:24]=[CH2:25])[CH2:7][CH:8]=[CH2:9])[CH:4]=[CH2:5].[Br-].[CH2:30]([CH:33]([NH2+:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH3:49])[CH2:34][CH:35]=[CH2:36])[CH:31]=[CH2:32].Cl.Cl.N(C(C)(C)C(N)=N)=NC(C)(C)C(N)=N>O>[Br-:1].[Br-:1].[CH2:3]([CH:6]([NH2+:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][NH2+:21][CH:22]([CH2:26][CH:27]=[CH2:28])[CH2:23][CH:24]=[CH2:25])[CH2:7][CH:8]=[CH2:9])[CH:4]=[CH2:5].[Br-:1].[CH2:30]([CH:33]([NH2+:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH2:48][CH3:49])[CH2:34][CH:35]=[CH2:36])[CH:31]=[CH2:32]

참가 물질

5

반응물 3

HCID 763442,2'-Azobis(2-methylpropanimidamide) dihydrochlorideHCID 219098721,10-Bis(diallylmethylammonio)decane DibromideHCID 86593797Diallylmethyldodecylammonium Bromide

생성물 1

HCID 865937981,10-bis(diallylmethylammonio)decane Dibromide Diallylmethyldodecylammonium Bromide수율 148.1%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

To a 500-mL round bottom flask was added 1,10-bis(diallylmethylammonio) decane dibromide (21.1 g), diallylmethyldodecylammonium bromide (21.1 g), and water (52 g). Azobisisobutyramidine dihydrochloride (1 mL of a 50% aqueous solution) was added and nitrogen was bubbled through the mixture for 1 hr. The mixture was then heated to 60° C. with stirring for 18 hr. The resulting gel was allowed to cool to room temperature. The gel was removed and ground in a blender with water (250 mL). The solid was collected by filtration and resuspended in methanol (250 mL). The solid was collected by filtration and resuspended in methanol (250 mL). After stirring for 1 hr, the solid was collected by filtration and resuspended in aqueous NaCl (250 mL of 1.5 M solution). After again stirring for 1 hr, the solid was collected by filtration. The aqueous NaCl rinse was repeated twice more, and the solid was rinsed with water until the conductivity of the rinse reached 0.08 mS/cm. The solid was dried in a forced-air oven at 60° C. to yield 17.6 g of product.

후처리

  1. customnitrogen was bubbled through the mixture for 1 hr
  2. temperatureto cool to room temperature
  3. customThe gel was removed
  4. filtrationThe solid was collected by filtration
  5. filtrationThe solid was collected by filtration
  6. stirringAfter stirring for 1 hr
  7. filtrationthe solid was collected by filtration
  8. stirringAfter again stirring for 1 hr
  9. filtrationthe solid was collected by filtration
  10. washThe aqueous NaCl rinse
  11. washthe solid was rinsed with water until the conductivity of the rinse
  12. customThe solid was dried in a forced-air oven at 60° C.

출처 및 근거

ORD 기록
ord-cc4f5fbf365343b29cfa2d6df90dda2a
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610283B1

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