Chloroform → Didecyldimethylammonium trans-Cinnamate

HRID 2403116

反応式

HRID 2403116 の反応式
[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]

参加物

6

反応物 3

HCID 6212ChloroformHCID 16958DidecyldimethylammoniumHCID 444539Cinnamic Acid

生成物 1

HCID 67382645Didecyldimethylammonium trans-Cinnamate収率 93%

試薬・触媒・溶媒 2

HCID 16957Didecyl dimethyl ammonium bromide触媒HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-659bb189dd2e4f7cbfb156ff5dd61d0a
出典データセット
uspto-grants-2014_08
特許番号
US08802596B2

関連ノート

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