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Potassium Acetate → Diethyl-2,5-bis-(10-acetoxydecoxy)terephthalate

HRID 378499
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HRID 378499 반응식
[CH2:1]([O:3][C:4](=[O:40])[C:5]1[CH:15]=[C:14]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]Br)[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][C:6]=1[O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38]Br)[CH3:2].[C:41]([O-:44])(=[O:43])[CH3:42].[K+]>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C(#N)C>[CH2:1]([O:3][C:4](=[O:40])[C:5]1[CH:15]=[C:14]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][O:43][C:41](=[O:44])[CH3:42])[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][C:6]=1[O:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][O:40][C:4](=[O:3])[CH3:5])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 517044Potassium AcetateHCID 19354090Diethyl-2,5-bis-(10-bromodecoxy)terephthalate

생성물 1

HCID 19354086Diethyl-2,5-bis-(10-acetoxydecoxy)terephthalate

시약·촉매·용매 2

HCID 21218Trioctylmethylammonium chloride촉매HCID 6342Acetonitrile용매

실험 절차

46.4 g (67.0 mmol) diethyl-2,5-bis-(10-bromodecoxy)terephthalate, 65.8 g (671 mmol) potassium acetate and 3.4 g (8.5 mmol) Aliquat 336® in 350 ml absolute acetonitrile are heated under N2 under reflux for 48 hours. After distilling off the solvent, the reaction mixture is taken up in 300 ml chloroform, insoluble salts are filtered off and the filtrate is washed twice with 150 ml water. The organic phase is dried over Na2SO4 and the solvent is then distilled off. 300 ml petroleum ether are added to the remaining, oily residue, the product crystallising out after 16 hours at -20° C. It is then recrystallized from ethanol.

후처리

  1. temperatureunder reflux for 48 hours
  2. distillationAfter distilling off the solvent
  3. filtrationinsoluble salts are filtered off
  4. washthe filtrate is washed twice with 150 ml water
  5. dry with materialThe organic phase is dried over Na2SO4
  6. distillationthe solvent is then distilled off
  7. addition300 ml petroleum ether are added to the remaining, oily residue
  8. customthe product crystallising out after 16 hours at -20° C
  9. customIt is then recrystallized from ethanol

출처 및 근거

ORD 기록
ord-98f4381273a6448eb0452d17566b6ca2
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06031015

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