Sulfuric Acid → 6-(22-Hydroxydocosyl)-2,3-dimethoxy-5-methylphenol

HRID 637885노트

반응식

HRID 637885 반응식
[OH:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([O:10][CH3:11])[CH:5]=[C:4]([CH3:12])[C:3]=1[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][C:34](OC)=[O:35].[H-].[Al+3].[Li+].[H-].[H-].[H-].S(=O)(=O)(O)O>O1CCCC1>[OH:35][CH2:34][CH2:33][CH2:32][CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25][CH2:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][C:3]1[C:2]([OH:1])=[C:7]([O:8][CH3:9])[C:6]([O:10][CH3:11])=[CH:5][C:4]=1[CH3:12]

참가 물질

5

반응물 3

HCID 1118Sulfuric AcidHCID 12824096HCID 12824096, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 128241256-(22-Hydroxydocosyl)-2,3-dimethoxy-5-methylphenol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of methyl 22-(2-hydroxy-3,4-dimethoxy-6-methylphenyl)docosanoate (3 g) in tetrahydrofuran (30 ml) is added lithium aluminum hydride and the mixture is stirred at room temperature for 1 hour. Under ice-cooling, 10% aqueous solution of sulfuric acid is added to the reaction mixture. The mixture is subjected to extraction with ether. The extract is washed with water and dried. The solvent is distilled off under reduced pressure, whereby 6-(22-hydroxydocosyl)-2,3-dimethoxy-5-methylphenol is obtained as colorless needles. m.p. 78° C.-81° C.

후처리

  1. temperatureUnder ice-cooling
  2. extractionThe mixture is subjected to extraction with ether
  3. washThe extract is washed with water
  4. customdried
  5. distillationThe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-91b74e34e9134ad19d30f0b636f29b2d
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04559177

반응 노트

불러오는 중…