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Methanol → HCID 57867352, 화합물

HRID 1516252
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HRID 1516252 반응식
C([O:9][CH2:10][C@@H:11]1[C@@H:15]([O:16]C(=O)C2C=CC=CC=2)[C@:14]([F:26])([CH3:25])[CH:13]([O:27][CH3:28])[O:12]1)(=O)C1C=CC=CC=1.CO>N>[F:26][C@@:14]1([CH3:25])[CH:13]([O:27][CH3:28])[O:12][C@H:11]([CH2:10][OH:9])[C@H:15]1[OH:16]
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참가 물질

4

반응물 2

HCID 887MethanolHCID 57867359HCID 57867359, 화합물

생성물 1

HCID 57867352HCID 57867352, 화합물수율 99%

시약·촉매·용매 1

HCID 222Ammonia용매

실험 절차

((2R,3R,4R)-3-benzoyloxy-4-fluoro-5-methoxy-4-methyl-tetrahydrofuran-2-yl)methyl benzoate (17 g, 43.8 mmol) in methanolic ammonia solution (25% w/w, 340 ml) was stirred at room temperature for about 36 hours, completion of the reaction monitored by thin-layer chromatography, methanol was removed under reduced pressure. Water added to the reaction mixture and extracted with ethyl acetate and the organic layer was dried over sodium sulphate. Concentration under reduced pressure and purification by silica gel column chromatography using 20% ethyl acetate in hexane eluded the title compound (8 g) as an off-white solid. Yield: 99%.

후처리

  1. customwas removed under reduced pressure
  2. additionWater added to the reaction mixture
  3. extractionextracted with ethyl acetate
  4. dry with materialthe organic layer was dried over sodium sulphate
  5. concentrationConcentration
  6. customunder reduced pressure and purification by silica gel column chromatography

출처 및 근거

ORD 기록
ord-e733548a843a4e7390bd7f79723532c1
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08227431B2

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