Hydrochloric Acid → 4-acetyl-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one

HRID 7883

반응식

HRID 7883 반응식
[CH2:1]([C:5]12[CH2:17][CH2:16][C:15](=[O:18])[C:14]([C:19]([O:21]CC)=[CH2:20])=[C:13]1[C:12]1[C:7](=[C:8]([Cl:26])[C:9]([O:24][CH3:25])=[CH:10][CH:11]=1)[CH2:6]2)[CH2:2][CH2:3][CH3:4].Cl>C(O)C.O>[C:19]([C:14]1[C:15](=[O:18])[CH2:16][CH2:17][C:5]2([CH2:1][CH2:2][CH2:3][CH3:4])[C:13]=1[C:12]1[C:7](=[C:8]([Cl:26])[C:9]([O:24][CH3:25])=[CH:10][CH:11]=1)[CH2:6]2)(=[O:21])[CH3:20]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 219909099a-butyl-8-chloro-4-(1-ethoxyvinyl)-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one

생성물 1

HCID 219908794-acetyl-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

The product from step 1 in ethanol (1.0 mL), water (0.2 mL) and aqueous 2N HCl (0.2 mL) was stirred and heated in an oil bath at 80° C. for 40 minutes. After cooling, the mixture was partitioned between EtOAc (20 mL) and water (20 mL). The organic phase was washed with brine (20 mL), dried over MgSO4, filtered, and evaporated under vacuum to provide 4-acetyl-9a-butyl-8-chloro-7-methoxy-1,2,9,9a-tetrahydro-3H-fluoren-3-one (54 mg) as an oil.

후처리

  1. temperatureAfter cooling
  2. customthe mixture was partitioned between EtOAc (20 mL) and water (20 mL)
  3. washThe organic phase was washed with brine (20 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-194006f950674b50a93e6edc19549752
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07087599B2

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