Dimethylformamide → Idebenone

HRID 637893

반응식

HRID 637893 반응식
CN(C)[CH:3]=[O:4].[OH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]1[C:22]([OH:23])=[C:21]([O:24][CH3:25])[C:20]([O:26][CH3:27])=[CH:19][C:18]=1C>O=O>[OH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][C:17]1[C:22](=[O:23])[C:21]([O:24][CH3:25])=[C:20]([O:26][CH3:27])[C:3](=[O:4])[C:18]=1[CH3:19]

참가 물질

4

반응물 2

HCID 6228DimethylformamideHCID 128241262-(10-Hydroxydecyl)-5,6-dimethoxy-3-methylphenol

생성물 1

HCID 3686Idebenone

시약·촉매·용매 1

HCID 977Oxygen용매

실험 절차

To a dimethylformamide solution (50 ml) of 6-(10-hydroxydecyl)-2,3-dimethoxy-5-methylphenol (2.53 g) is added bis(salicylidene)ethylenediiminocobalt(II) (salcomine) (0.1 g) and the mixture is stirred in oxygen streams at atmospheric temperature and pressure for 72 hours. The solvent is then distilled off and the product is extracted with ether. The ethereal layer is washed with water and dried over anhydrous sodium sulfate, and the solvent is distilled off. The above procedure yields 6-(10-hydroxydecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (2.32 g) as orange-yellow needles melting at 52° C.

후처리

  1. distillationThe solvent is then distilled off
  2. extractionthe product is extracted with ether
  3. washThe ethereal layer is washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent is distilled off

출처 및 근거

ORD 기록
ord-89389e2d066544e2a89c18db6e62ed8f
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559177

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