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

HRID 397223

反応式

HRID 397223 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-cc4f5fbf365343b29cfa2d6df90dda2a
出典データセット
uspto-grants-2003_08
特許番号
US06610283B1

関連ノート

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