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Potassium Carbonate → HCID 69112481, 화합물

HRID 2228837
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HRID 2228837 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][C@H:8]1[CH2:13][C@H:12]([O:14][Si:15]([C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:17])[CH3:16])[CH2:11][C@@H:10](CC([O-])=O)[CH2:9]1.C(=O)([O-])[O-:27].[K+].[K+]>CO>[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][C@H:8]1[CH2:13][C@H:12]([O:14][Si:15]([C:18]([CH3:21])([CH3:20])[CH3:19])([CH3:17])[CH3:16])[CH2:11][C@@H:10]([OH:27])[CH2:9]1
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참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 86758332HCID 86758332, 화합물

생성물 1

HCID 69112481HCID 69112481, 화합물수율 96%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3-tetrahydro-2H-2-pyranyloxy-5-(tert.butyldimethylsilyloxy)-(1S,3R,5R)-cyclohexylacetate (6, 3.5 parts, 9.16 mmol) was dissolved in dry methanol (25 parts). To the solution anhydrous potassium carbonate (0.828 parts, 6 mmol) was added and the mixture was stirred at room temperature for 2 hr. Methanol was removed under vacuum and residue was extracted several times with dichloromethane. Dichloromethane layers were combined and washed with water followed by brine wash. It was dried on anhydrous sodium sulfate. Solvent was removed under vacuum and residue was purified by flash column chromatography to yield 3-tetrahydro-2H-2-pyranyloxy-5-(tert.butyldimethylsilyloxy)-(1S,3R,5R)-cyclohexan-1-ol (7, yield 3 parts, 96%).

후처리

  1. customMethanol was removed under vacuum and residue
  2. extractionwas extracted several times with dichloromethane
  3. washwashed with water
  4. washwash
  5. dry with materialIt was dried on anhydrous sodium sulfate
  6. customSolvent was removed under vacuum and residue
  7. customwas purified by flash column chromatography

출처 및 근거

ORD 기록
ord-cf2ea5c85efe431f82112f218757e0b1
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06417374B1

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