Chloroform → Didecyldimethylammonium trans-Cinnamate

HRID 1517213

반응식

HRID 1517213 반응식
[C:1]([OH:11])(=[O:10])/[CH:2]=[CH:3]/[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH2:12]([N+:22]([CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH3:34])([CH3:24])[CH3:23])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21].C(Cl)(Cl)Cl>[Br-].C([N+](CCCCCCCCCC)(C)C)CCCCCCCCC.CS(C)=O>[C:1]([O-:11])(=[O:10])/[CH:2]=[CH:3]/[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.[CH2:25]([N+:22]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])([CH3:24])[CH3:23])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH3:34]

참가 물질

6

반응물 3

HCID 6212ChloroformHCID 16958DidecyldimethylammoniumHCID 444539Cinnamic Acid

생성물 1

HCID 67382645Didecyldimethylammonium trans-Cinnamate수율 93%

시약·촉매·용매 2

HCID 16957Didecyl dimethyl ammonium bromide촉매HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
90 °C

실험 절차

Didecyldimethylammonium bromide (0.001 mol) was dissolved in 50 mL of hot distilled water. trans-Cinnamic acid (0.001 mol) was added to the didecyldimethylammonium solution. The reaction solution was stirred at 90° C. for 4 h. The reaction solution was cooled to room temperature and then 60 mL of chloroform was added. The two phases were separated and the chloroform phase was washed several times with cool distilled water to remove any inorganic salt. The presence of chloride anions was monitored by silver nitrate test. A rotary evaporator removed the chloroform and a wax was obtained in 93% yield. 1H and 13C NMR (DMSO) were obtained. Melting point (hot plate apparatus)=54-55° C.

후처리

  1. distillationof hot distilled water
  2. temperatureThe reaction solution was cooled to room temperature
  3. customThe two phases were separated
  4. washthe chloroform phase was washed several times
  5. temperaturewith cool
  6. distillationdistilled water
  7. customto remove any inorganic salt
  8. customA rotary evaporator
  9. customremoved the chloroform
  10. customa wax was obtained in 93% yield
  11. customMelting point (hot plate apparatus)=54-55° C.

출처 및 근거

ORD 기록
ord-07bc9591767e4647ad69c355dd98f823
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232265B2

연결된 노트

불러오는 중…