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

HRID 2389930ノート

反応式

HRID 2389930 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-157098d007ad4fa488254263c3ffa623
出典データセット
uspto-grants-2012_09
特許番号
US08273761B2

反応ノート

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