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N-(3-Chloropropyl)-N,N-dimethyl-1-dodecanaminium bromide → N-(N,N-dimethyl-N-dodecylammonio) propyldiallylmethylammonium Chloride Bromide

HRID 1532522
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HRID 1532522 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][N+:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])([CH3:16])[CH3:15]>CO>[Br-:9].[Cl-:10].[CH3:15][N+:14]([CH2:13][CH2:12][CH2:11][NH2+:8][CH:4]([CH2:5][CH:6]=[CH2:7])[CH2:1][CH:2]=[CH2:3])([CH3:16])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]
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참가 물질

4

반응물 2

HCID 10861601N-(3-Chloropropyl)-N,N-dimethyl-1-dodecanaminium bromideHCID 12791689Hepta-1,6-dien-4-amine

생성물 1

HCID 86593801N-(N,N-dimethyl-N-dodecylammonio) propyldiallylmethylammonium Chloride Bromide수율 73.4%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
65 °C

실험 절차

A mixture of 22 g diallylmethylamine and 74 g 3-chloropropyldodecyldimethylammonium 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 dialllymethylamine 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 70 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-4c6acf801def4382b6149557782ee592
출처 데이터셋
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06203785B1

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