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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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3,4-dihydro-2H-pyran → (3aR, 4R, 5R, 6aS) Hexahydro-4-[(E)-(3S)-5-phenyl-3-(tetrahydropyran-2-yloxy)-1-pentenyl]-5-(tetrahydropyran-2-yloxy)-2H-cyclopenta[b]furan-2-one

HRID 517401
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HRID 517401 반응식
[OH:1][C@@H:2]1[CH2:10][C@@H:5]2[O:6][C:7](=[O:9])[CH2:8][C@@H:4]2[C@H:3]1/[CH:11]=[CH:12]/[C@@H:13]([OH:22])[CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[O:23]1[CH:28]=[CH:27][CH2:26][CH2:25][CH2:24]1.[C:29](=[O:32])(O)[O-].[Na+]>ClCCl.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:16]1([CH2:15][CH2:14][C@H:13]([O:22][CH:4]2[CH2:3][CH2:2][CH2:10][CH2:29][O:32]2)/[CH:12]=[CH:11]/[C@@H:3]2[C@@H:4]3[C@@H:5]([O:6][C:7](=[O:9])[CH2:8]3)[CH2:10][C@H:2]2[O:1][CH:28]2[CH2:27][CH2:26][CH2:25][CH2:24][O:23]2)[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 80803,4-dihydro-2H-pyranHCID 516892Sodium BicarbonateHCID 13046417HYDRIDE-L

생성물 1

HCID 11102745(3aR, 4R, 5R, 6aS) Hexahydro-4-[(E)-(3S)-5-phenyl-3-(tetrahydropyran-2-yloxy)-1-pentenyl]-5-(tetrahydropyran-2-yloxy)-2H-cyclopenta[b]furan-2-one수율 89.9%

시약·촉매·용매 2

HCID 521998
p-Toluenesulfonic acid monohydrate
촉매
HCID 6344Dichloromethane용매

실험 절차

p-Toluenesulfonic acid monohydrate (0.3 g, 0.165 mmol) was added to a solution of (3aR,4R,5R,6aS)-hexahydro-5-hydroxy-4-((S,E)-3-hydroxy-5-phenylpent-1-enyl)cyclopenta[b]furan-2-one (10.0 g, 33.1 mmol) and 3,4-dihydro-2H-pyran (4.2 g, 49.7 mmol) in dichloromethane (100 mL) at room temperature and the mixture was stirred for 2.5 hr (TLC monitoring). Saturated aqueous solution of sodium bicarbonate (100 mL) was poured into the reaction mixture and the mixture was stirred for 5 minutes. The organic layer was separated and the aqueous layer was extracted with ethyl acetate (100 mL). The combined organic layers were dried over magnesium sulfate, the solid was filtered off and the filtrate was concentrated under reduced pressure to give 16.0 g of crude product. The crude product was purified by column chromatography and then concentrated under reduced pressure to provide 14.0 g of the title compound (89.9% yield).

후처리

  1. stirringthe mixture was stirred for 5 minutes
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with ethyl acetate (100 mL)
  4. dry with materialThe combined organic layers were dried over magnesium sulfate
  5. filtrationthe solid was filtered off
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customto give 16.0 g of crude product
  8. customThe crude product was purified by column chromatography
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-09ac1a3581ec4afab06de3b6d779e0fe
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115109B2

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