5-(3-Methyloctan-2-yl)benzene-1,3-diol → 1,2-Dihydro-2,2-dimethyl-9-hydroxy-7-(3-methyl-2-octyl)-4-oxo-4H-thieno-[2,3-c][1] benzopyran

HRID 268119

반응식

HRID 268119 반응식
[CH3:1][CH:2]([CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:3]([C:5]1[CH:6]=[C:7]([OH:12])[CH:8]=[C:9]([CH:11]=1)[OH:10])[CH3:4].[CH3:18][C:19]1([CH3:30])[S:23][CH:22]([C:24](OCC)=[O:25])[C:21](=O)[CH2:20]1>C(O)C>[CH3:18][C:19]1([CH3:30])[S:23][C:22]2[C:24](=[O:25])[O:10][C:9]3[CH:11]=[C:5]([CH:3]([CH:2]([CH3:1])[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH3:4])[CH:6]=[C:7]([OH:12])[C:8]=3[C:21]=2[CH2:20]1

참가 물질

4

반응물 2

HCID 2581765-(3-Methyloctan-2-yl)benzene-1,3-diolHCID 12716257Ethyl 5,5-dimethyl-3-oxothiolane-2-carboxylate

생성물 1

HCID 215200041,2-Dihydro-2,2-dimethyl-9-hydroxy-7-(3-methyl-2-octyl)-4-oxo-4H-thieno-[2,3-c][1] benzopyran

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 100 ml. of ethanol was added 6.2 g. of 5-(3-methyl-2-octyl)resorcinol and 6.2 g. of ethyl 5,5-dimethyl-3-oxotetrahydrothiophene-2-carboxylate. The mixture was cooled in ice and hydrogen chloride was bubbled in for one-half hour. The mixture was stoppered and held at room temperature for 3 days. It was then concentrated and ether added, extracted with water and then washed with dilute aqueous sodium bicarbonate solution. The etheral solution was dried over magnesium sulfate and concentrated. The product was crystallized from acetonitrile to give 5.0 g., m.p. 155°-163°C.

후처리

  1. temperatureThe mixture was cooled in ice
  2. customhydrogen chloride was bubbled in for one-half hour
  3. concentrationIt was then concentrated
  4. additionether added
  5. extractionextracted with water
  6. washwashed with dilute aqueous sodium bicarbonate solution
  7. dry with materialThe etheral solution was dried over magnesium sulfate
  8. concentrationconcentrated
  9. customThe product was crystallized from acetonitrile
  10. customto give 5.0 g

출처 및 근거

ORD 기록
ord-098fcb95100841839e3f9fed4f971686
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03946111

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