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Water → 9a-Acetyl-1,2,3,4,4a,9a-hexahydrofluoren-9-one

HRID 279146
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HRID 279146 반응식
[CH2:1]1[CH:13]2[CH:5]([C:6]3[C:11]([C:12]2=[O:14])=[CH:10][CH:9]=[CH:8][CH:7]=3)[CH2:4][CH2:3][CH2:2]1.[C:15]1([CH3:25])C=CC(S(O)(=O)=O)=CC=1.[OH2:26]>C(OC(=O)C)(=O)C>[C:15]([C:11]12[CH2:10][CH2:9][CH2:8][CH2:7][CH:6]1[C:5]1[C:13](=[CH:1][CH:2]=[CH:3][CH:4]=1)[C:12]2=[O:14])(=[O:26])[CH3:25]
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참가 물질

5

반응물 3

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 6041812,3,4,4a-Tetrahydro-1H-fluoren-9(9aH)-one

생성물 1

HCID 226245739a-Acetyl-1,2,3,4,4a,9a-hexahydrofluoren-9-one

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

1,2,3,4,4a,9a-Hexahydrofluoren-9-one (9.6 g) was dissolved in acetic anhydride (40 ml). p-Toluenesulfonic acid (1 g) was added and the mixture was refluxed for 1 hour. The mixture was cooled in an ice bath and water (20 ml) was added. After stirring for 20 minutes solvent was removed with an evaporator. The residue was dissolved in ethyl acetate (60 ml) and extracted with 5% NaHCO3 solution (2×30 ml) and water (30 ml). The organic phase was dried over Na2SO4 and evaporated. Yield was 10.9 g.

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperatureThe mixture was cooled in an ice bath
  3. customwas removed with an evaporator
  4. dissolutionThe residue was dissolved in ethyl acetate (60 ml)
  5. extractionextracted with 5% NaHCO3 solution (2×30 ml) and water (30 ml)
  6. dry with materialThe organic phase was dried over Na2SO4
  7. customevaporated

출처 및 근거

ORD 기록
ord-d319a0a5a2fc484d94ec9b3b85b624bd
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06362211B1

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