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Methanol → HCID 86201264, 화합물

HRID 2270557
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HRID 2270557 반응식
C([O:3][C:4](=O)[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[C:6]=1[O:14][CH2:15][CH3:16])C.O1CCCC1.CO.[BH4-].[Li+]>O>[CH2:15]([O:14][C:6]1[C:7]([N+:11]([O-:13])=[O:12])=[CH:8][CH:9]=[CH:10][C:5]=1[CH2:4][OH:3])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 8028TetrahydrofuranHCID 4148881Lithium borohydrideHCID 54007593HCID 54007593, 화합물

생성물 1

HCID 86201264HCID 86201264, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of the compound (117 mg) obtained in Example 417a, tetrahydrofuran (5 ml) and methanol (2 ml), lithium borohydride (10.7 mg) was added. The reaction mixture was stirred at room temperature for 15 h, and, after addition of water, concentrated under reduced pressure. To the resulting residue, 2 N HCl was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate:n-hexane=1:2) to give the titled compound quantitatively.

후처리

  1. additionwas added
  2. concentrationconcentrated under reduced pressure
  3. additionTo the resulting residue, 2 N HCl was added
  4. extractionthe mixture was subjected to extraction with ethyl acetate
  5. washThe organic layer was washed with a saturated aqueous sodium chloride solution
  6. dry with materialdried with anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate:n-hexane=1:2)

출처 및 근거

ORD 기록
ord-cf682594faad4d5d82d93ab8fc3530a7
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06331553B1

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