Sodium sulfate decahydrate → (2-Ethyl-8,9-dihydrofuro[3,2-c]pyrazolo[1,5-a]pyridin-1-yl)methanol

HRID 2389878ノート

反応式

HRID 2389878 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([C:9]1[C:20]([C:21](OCC)=[O:22])=[C:12]2[C:13]3[CH2:19][CH2:18][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:20]([CH2:21][OH:22])=[C:12]2[C:13]3[CH2:19][CH2:18][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 53310990Ethyl 2-ethyl-8,9-dihydrofuro[3,2-c]pyrazolo[1,5-a]pyridine-1-carboxylate

生成物 1

HCID 53308851(2-Ethyl-8,9-dihydrofuro[3,2-c]pyrazolo[1,5-a]pyridin-1-yl)methanol収率 75.1%

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 (548 mg, 11.8 mmol) in tetrahydrofuran (30 mL) was added a solution of ethyl 2-ethyl-8,9-dihydrofuro[3,2-c]pyrazolo[1,5-a]pyridine-1-carboxylate (770 mg, 2.96 mmol) in tetrahydrofuran (30 mL) under ice-cooling, and the mixture was stirred at room temperature for 30 min. Sodium sulfate decahydrate (10 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 (485 mg, yield 75%).

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-5083c956ec1f434783ea5c6f29c274ea
出典データセット
uspto-grants-2012_09
特許番号
US08273761B2

反応ノート

読み込み中…