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Sodium sulfate decahydrate → (2-Phenylfuro[3,2-c]pyrazolo[1,5-a]pyridin-1-yl)methanol

HRID 2389876
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HRID 2389876 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C:13]2[C:24]([C:25](OC)=[O:26])=[C:16]3[C:17]4[CH:23]=[CH:22][O:21][C:18]=4[CH:19]=[CH:20][N:15]3[N:14]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[C:7]1([C:13]2[C:24]([CH2:25][OH:26])=[C:16]3[C:17]4[CH:23]=[CH:22][O:21][C:18]=4[CH:19]=[CH:20][N:15]3[N:14]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
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참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 59179362Methyl 2-phenylfuro[3,2-c]pyrazolo[1,5-a]pyridine-1-carboxylate

생성물 1

HCID 59179389(2-Phenylfuro[3,2-c]pyrazolo[1,5-a]pyridin-1-yl)methanol수율 87.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
50 °C

실험 절차

To a suspension of 80% lithium aluminum hydride (294 mg, 6.35 mmol) in tetrahydrofuran (10 mL) was added a solution of methyl 2-phenylfuro[3,2-c]pyrazolo[1,5-a]pyridine-1-carboxylate (465 mg, 1.59 mmol) in tetrahydrofuran (10 mL) at room temperature, and the mixture was stirred at 50° C. for 5 min. Sodium sulfate decahydrate (4.3 g) was added under ice-cooling, and the insoluble material was filtered off. The filtrate was concentrated under reduced pressure and the residue was purified by recrystallization (ethyl acetate) to give the title compound (367 mg, yield 87%).

후처리

  1. temperaturecooling
  2. filtrationthe insoluble material was filtered off
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by recrystallization (ethyl acetate)

출처 및 근거

ORD 기록
ord-494313a2683f4ff6b67b55e9269d5ba9
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08273761B2

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