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

HRID 378498

反応式

HRID 378498 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8771b1594f4a446fb4425ec5b0c79c75
出典データセット
uspto-grants-2000_02
特許番号
US06031015

関連ノート

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