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Sulfuric Acid → (+)-(4S,5R)-3,4-Dihydroxy-2-(3-methylbutanoyl)-5-(3-methylbutyl)-4-(4-methylpentanoyl)cyclopent-2-en-1-one

HRID 1959331
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HRID 1959331 반응식
[CH3:1][CH:2]([CH2:4][C:5]([C:7]1[C:11](=[O:12])[C@@H:10]([CH2:13][CH:14]=[C:15]([CH3:17])[CH3:16])[C@:9]([OH:25])([C:18]([CH2:20][CH:21]=[C:22]([CH3:24])[CH3:23])=[O:19])[C:8]=1[OH:26])=[O:6])[CH3:3].[H][H].S(=O)(=O)(O)O>CO.[Pd]>[CH3:17][CH:15]([CH2:14][CH2:13][C@@H:10]1[C@@:9]([OH:25])([C:18]([CH2:20][CH2:21][CH:22]([CH3:23])[CH3:24])=[O:19])[C:8]([OH:26])=[C:7]([C:5]([CH2:4][CH:2]([CH3:3])[CH3:1])=[O:6])[C:11]1=[O:12])[CH3:16]
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참가 물질

6

반응물 3

HCID 1118Sulfuric AcidHCID 21594782Isohumulone, cis-(+)-HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 56956246(+)-(4S,5R)-3,4-Dihydroxy-2-(3-methylbutanoyl)-5-(3-methylbutyl)-4-(4-methylpentanoyl)cyclopent-2-en-1-one

시약·촉매·용매 2

HCID 23938Palladium촉매
HCID 887
Methanol
용매

실험 절차

96.3 mg of the dry Mg salt of (+)-cis isohumulone ((+)-VIII) was dissolved in 1 mL of methanol. 3.1 mg (0.3 eq) of MgO was added, and the reaction mixture was stirred for five minutes. 30 mg of 10% Pd/C was added to the solution, and stirring was resumed. A hydrogen atmosphere was introduced by bubbling hydrogen gas into the solution. After 45 minutes the reaction was judged to be complete by HPLC, the stirring was stopped, and the hydrogen atmosphere was removed by opening the vial. 1 equivalent of sulfuric acid was added to the reaction mixture (pH ˜1), and the reaction was filtered through a 0.2 mm syringe filter. The reaction vessel and filter were washed 2 times successively with ethyl acetate. The filtrate was concentrated in vacuo, redissolved in hexanes, dried over Na2SO4, filtered via a cotton pipette, and concentrated in vacuo and dried overnight at 0.070 mbar. 58.1 mg of (+)-KDT-500 was produced. Further purification was carried out via chromatography and crystallization.

후처리

  1. stirringstirring
  2. customby bubbling hydrogen gas into the solution
  3. waitAfter 45 minutes the reaction was judged
  4. customthe hydrogen atmosphere was removed
  5. filtrationthe reaction was filtered through a 0.2 mm syringe
  6. filtrationfilter
  7. filtrationThe reaction vessel and filter
  8. washwere washed 2 times successively with ethyl acetate
  9. concentrationThe filtrate was concentrated in vacuo
  10. dissolutionredissolved in hexanes
  11. dry with materialdried over Na2SO4
  12. filtrationfiltered via a cotton pipette
  13. concentrationconcentrated in vacuo
  14. customdried overnight at 0.070 mbar

출처 및 근거

ORD 기록
ord-e106d20898d84bf282961ff7f241bae4
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08410178B2

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