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Acetyl chloride → N-[2-(1,6,7,8-tetrahydro-2H-cyclopenta[b]furo[3,2-d]pyridin-8-yl)ethyl]acetamide

HRID 2389942
ノート
印刷プレビュー

反応式

HRID 2389942 の反応式
[CH2:1]1[C:5]2=[C:6]3[C:7]([CH2:10][CH2:11]/[C:12]/3=[CH:13]\[CH2:14][NH2:15])=[N:8][CH:9]=[C:4]2[O:3][CH2:2]1.[C:16](Cl)(=[O:18])[CH3:17]>N1C=CC=CC=1.C(=O)([O-])O.[Na+]>[CH2:1]1[C:5]2=[C:6]3[CH:12]([CH2:13][CH2:14][NH:15][C:16](=[O:18])[CH3:17])[CH2:11][CH2:10][C:7]3=[N:8][CH:9]=[C:4]2[O:3][CH2:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6367Acetyl chlorideHCID 59179360(2E)-2-(1,2,6,7-tetrahydro-8H-cyclopenta[b]furo[3,2-d]pyridin-8-ylidene)ethanamine

生成物 1

HCID 59179455N-[2-(1,6,7,8-tetrahydro-2H-cyclopenta[b]furo[3,2-d]pyridin-8-yl)ethyl]acetamide収率 22%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

To a solution of (2E)-2-(1,2,6,7-tetrahydro-8H-cyclopenta[b]furo[3,2-d]pyridin-8-ylidene)ethanamine (186 mg, 0.920 mmol) in pyridine (3.7 mL) was added acetyl chloride (78.5 μL, 1.10 mmol) under ice-cooling, and the mixture was stirred for 10 min. The reaction solution was diluted with saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=50/50→100/0). The residue was dissolved in methanol (1.1 mL), palladium-carbon powder (11 mg) was added, and the mixture was stirred at 50° C. for 3 hr under a hydrogen atmosphere. The catalyst was filtered off, and the filtrate was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane=90/10→100/0) to give the title compound (49.1 mg, yield 22%).

後処理

  1. temperaturecooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane=50/50→100/0)
  6. dissolutionThe residue was dissolved in methanol (1.1 mL)
  7. additionpalladium-carbon powder (11 mg) was added
  8. stirringthe mixture was stirred at 50° C. for 3 hr under a hydrogen atmosphere
  9. filtrationThe catalyst was filtered off
  10. customthe filtrate was evaporated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane=90/10→100/0)

出典と根拠

ORDレコード
ord-a4076a7182154e91b594e3ae7b481a92
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273761B2

反応ノート

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