Dimethylformamide → Idebenone

HRID 637894

反応式

HRID 637894 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 3686Idebenone

試薬・触媒・溶媒 1

HCID 977Oxygen溶媒

実験手順

To a dimethylformamide solution (100 ml) of 6-(10-hydroxydecyl)-2,3-dimethoxy-5-methylphenol (4.1 g) is added bis(3-methoxysalicylidene)ethylenediiminocobalt(II) (0.2 g) and the mixture is stirred in oxygen streams at atmospheric temperature and pressure for 72 hours. After the reaction has been completed, the solvent is distilled off and the residue is extracted with ether. The ethereal layer is washed with water and dried, and the solvent is distilled off in the conventional manner. The crude crystals thus obtained are recrystallized from ethyl acetate-hexane (1:3). The above procedure yields 6-(10-hydroxydecyl)-2,3-dimethoxy-5-methyl-1,4-benzoquinone (3.77 g) as orange-yellow needles melting at 52° C.-53° C.

後処理

  1. distillationthe solvent is distilled off
  2. extractionthe residue is extracted with ether
  3. washThe ethereal layer is washed with water
  4. customdried
  5. distillationthe solvent is distilled off in the conventional manner
  6. customThe crude crystals thus obtained
  7. customare recrystallized from ethyl acetate-hexane (1:3)

出典と根拠

ORDレコード
ord-c74e2c1dabb34e8eaa8b99a4b3f84ac1
出典データセット
uspto-grants-1985_12
特許番号
US04559177

関連ノート

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