Pyridinium chloride → 3,4-Dichloro-6,7,8,8a,9,10-hexahydro-2-hydroxy-6-oxo-8a-propylphenanthrene

HRID 867995노트

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HRID 867995 반응식
Cl.N1C=CC=CC=1.[Cl:8][C:9]1[C:10]([O:28]CC(O)=O)=[CH:11][C:12]2[CH2:13][CH2:14][C:15]3([CH2:25][CH2:26][CH3:27])[C:20]([C:21]=2[C:22]=1[Cl:23])=[CH:19][C:18](=[O:24])[CH2:17][CH2:16]3>>[Cl:8][C:9]1[C:10]([OH:28])=[CH:11][C:12]2[CH2:13][CH2:14][C:15]3([CH2:25][CH2:26][CH3:27])[C:20]([C:21]=2[C:22]=1[Cl:23])=[CH:19][C:18](=[O:24])[CH2:17][CH2:16]3

참가 물질

3

반응물 2

HCID 10176127Pyridinium chlorideHCID 21289572[(3,4-Dichloro-6,7,8,8a,9,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]acetic acid

생성물 1

HCID 212895743,4-Dichloro-6,7,8,8a,9,10-hexahydro-2-hydroxy-6-oxo-8a-propylphenanthrene

반응 조건

온도
190 °C

실험 절차

Pyridine hydrochloride (20 g, 173 mmole) is melted and heated to 190° C. and then (-) [(3,4-dichloro-6,7,8,8a,9,10-hexahydro-6-oxo-8a-propyl-2-phenanthrenyl)oxy]acetic acid (Example 3) (325 mg, 1 mmole) is added and stirred for 15 minutes at 190°. The mixture is poured into crushed ice (200 g) and the product extracted with ether. The organic extract is washed with water, then with brine and dried over MgSO4. Evaporation of the solvent gave (-)3,4-dichloro-6,7,8,8a,9,10-hexahydro-2-hydroxy-6-oxo-8a-propylphenanthrene.

후처리

  1. additionThe mixture is poured
  2. extractionthe product extracted with ether
  3. extractionThe organic extract
  4. washis washed with water
  5. dry with materialwith brine and dried over MgSO4
  6. customEvaporation of the solvent

출처 및 근거

ORD 기록
ord-6e5d09f047a84d7e97034c1665a36b51
출처 데이터셋
uspto-grants-1988_10
특허 번호
US04777281

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