Sodium sulfate decahydrate → 2-Ethyl-8-methylfuro[3,2-c]pyrazolo[1,5-a]pyridine-1-methanol

HRID 2389930노트

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HRID 2389930 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([C:9]1[C:21]([C:22](OCC)=[O:23])=[C:12]2[C:13]3[CH:19]=[C:18]([CH3:20])[O:17][C:14]=3[CH:15]=[CH:16][N:11]2[N:10]=1)[CH3:8].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH2:7]([C:9]1[C:21]([CH2:22][OH:23])=[C:12]2[C:13]3[CH:19]=[C:18]([CH3:20])[O:17][C:14]=3[CH:15]=[CH:16][N:11]2[N:10]=1)[CH3:8]

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 59179437Ethyl 2-ethyl-8-methylfuro[3,2-c]pyrazolo[1,5-a]pyridine-1-carboxylate

생성물 1

HCID 591794472-Ethyl-8-methylfuro[3,2-c]pyrazolo[1,5-a]pyridine-1-methanol수율 124.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of 80% lithium aluminum hydride (293 mg, 7.91 mmol) in tetrahydrofuran (16 mL) was added a solution of ethyl 2-ethyl-8-methylfuro[3,2-c]pyrazolo[1,5-a]pyridine-1-carboxylate (430 mg, 1.26 mmol) in tetrahydrofuran (16 mL) under ice-cooling, and the mixture was stirred at room temperature for 30 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 washed with diisopropyl ether to give the title compound (360 mg, yield 99%).

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. filtrationthe insoluble material was filtered off
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. washthe residue was washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-157098d007ad4fa488254263c3ffa623
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08273761B2

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