Sodium Iodide → Diethyl-2,5-bis-(10-bromodecoxy)terephthalate

HRID 378498

반응식

HRID 378498 반응식
[CH2:1]([O:3][C:4](=[O:18])[C:5]1[CH:15]=[C:14]([OH:16])[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][C:6]=1[OH:17])[CH3:2].Br[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][Br:30].C([O-])([O-])=O.[K+].[K+].[Na+].[I-]>CC(C)=O>[CH2:1]([O:3][C:4](=[O:18])[C:5]1[CH:15]=[C:14]([O:16][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][Br:30])[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:7][C:6]=1[O:17][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][Br:30])[CH3:2]

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 79980Diethyl 2,5-dihydroxyterephthalateHCID 2214831,10-Dibromodecane

생성물 1

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

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

25.4 g (0.1 mol) diethyl-2,5-dihydroxyterephthalate, 450 g (1.5 mol) 1,10-dibromodecane, 138 g (1.0 mol) K2CO3 and 200 mg NaI in 200 ml acetone are heated under reflux for 28 hours until the originally yellow suspension has decolorized. After distilling off the solvent, the reaction mixture is extracted twice with diethyl ether (2×250 ml), and insoluble salts are filtered off. The filtrate is washed twice with 200 ml water and dried over Na2SO4. The solvent is then distilled off. The colourless, solid residue is washed twice with petroleum ether and then recrystallized from petroleum ether.

후처리

  1. temperatureunder reflux for 28 hours until the originally yellow suspension
  2. distillationAfter distilling off the solvent
  3. extractionthe reaction mixture is extracted twice with diethyl ether (2×250 ml), and insoluble salts
  4. filtrationare filtered off
  5. washThe filtrate is washed twice with 200 ml water
  6. dry with materialdried over Na2SO4
  7. distillationThe solvent is then distilled off
  8. washThe colourless, solid residue is washed twice with petroleum ether
  9. customrecrystallized from petroleum ether

출처 및 근거

ORD 기록
ord-8771b1594f4a446fb4425ec5b0c79c75
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06031015

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