Hepta-1,6-dien-4-amine → N-(N,N-Dimethyl-N-dodecylammonio)butyldiallylmethylammonium Chloride Bromide

HRID 397227

반응식

HRID 397227 반응식
[CH2:1]([CH:4]([NH2:8])[CH2:5][CH:6]=[CH2:7])[CH:2]=[CH2:3].[Br-:9].[Cl:10][CH2:11][CH2:12][CH2:13][CH2:14][N+:15]([CH3:29])([CH3:28])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]>CO>[Br-:9].[Cl-:10].[CH3:28][N+:15]([CH2:14][CH2:13][CH2:12][CH2:11][NH2+:8][CH:4]([CH2:5][CH:6]=[CH2:7])[CH2:1][CH:2]=[CH2:3])([CH3:29])[CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]

참가 물질

4

반응물 2

HCID 12791689Hepta-1,6-dien-4-amine2회HCID 158701334-Chlorobutyldimethyldodecylammonium bromide

생성물 1

HCID 86593803N-(N,N-Dimethyl-N-dodecylammonio)butyldiallylmethylammonium Chloride Bromide수율 67.2%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
65 °C

실험 절차

A mixture of 22 g diallylmethylamine and 75 g 4-chlorobutyldimethyldodecyl-ammonium bromide were dissolved in 100 mL methanol and the reaction mixture was stirred at 65° C. for 48 hours. The progress of the reaction was monitored by the disappearance of the diallylmethylamine by thin layer chromatography (TLC). After cooling to room temperature, the solvent was removed under reduced pressure. The residual viscous oil was precipitated into 800 mL dry ether with rapid stirring. The ether layer was decanted and the residue was again treated with 500 mL dry ether. After stirring for 15 minutes the solvent was removed and the oily residue was dried under vacuum at 35° C. for 48 hours, yielding 65 g of the product.

후처리

  1. temperatureAfter cooling to room temperature
  2. customthe solvent was removed under reduced pressure
  3. customThe residual viscous oil was precipitated into 800 mL dry ether with rapid stirring
  4. customThe ether layer was decanted
  5. additionthe residue was again treated with 500 mL dry ether
  6. stirringAfter stirring for 15 minutes the solvent
  7. customwas removed
  8. customthe oily residue was dried under vacuum at 35° C. for 48 hours

출처 및 근거

ORD 기록
ord-ca68ff58234a4e23b8c52b21d7ba058e
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610283B1

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