Tetrahydrofuran → HCID 57705499, 화합물

HRID 1662412노트

반응식

HRID 1662412 반응식
[CH3:1][C:2]([Si:5]([CH3:30])([CH3:29])[O:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:15]=2[F:22])=[C:10]([C:23](=[O:28])[C:24]([CH3:27])([CH3:26])[CH3:25])[CH:9]=1)([CH3:4])[CH3:3].C1COCC1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[OH-].[Na+]>>[CH3:4][C:2]([Si:5]([CH3:29])([CH3:30])[O:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:15]=2[F:22])=[C:10]([CH:23]([OH:28])[C:24]([CH3:27])([CH3:26])[CH3:25])[CH:9]=1)([CH3:1])[CH3:3]

참가 물질

5

반응물 4

HCID 8028Tetrahydrofuran2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 57706379HCID 57706379, 화합물

생성물 1

HCID 57705499HCID 57705499, 화합물수율 80%

실험 절차

To a stirred solution of 66.30A (0.500 g, 1.2 mmol) in THF (15.00 mL, 183 mmol) at 0° C. was added LAH in THF (2.3 mL, 2.3 mmol, 1.0M). The reaction was stirred for two hours. 1N NaOH(aq) was added to quench the reaction mixture, and the reaction was then extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and the product was then purified on silica gel (0-10% EtOAc in hexanes) to yield 66.30B as a colorless oil (0.400 g, 80% yield).

후처리

  1. customto quench the reaction mixture
  2. extractionthe reaction was then extracted three times with EtOAc
  3. dry with materialAfter drying over anhydrous magnesium sulfate
  4. filtrationfiltering
  5. customthe organic solvent was removed under reduced pressure
  6. customthe product was then purified on silica gel (0-10% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-d3ca36ddca474aefbf9febfd27df7790
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030354B2

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