Acetic Anhydride → N-[2-(2-methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethyl]acetamide

HRID 887799

反応式

HRID 887799 の反応式
[CH3:1][N:2]1[CH:10]=[C:9]2[C:4]([CH:5]=[CH:6][C:7]3[CH2:13][CH2:12][C:11](=[CH:14][CH2:15][NH2:16])[C:8]=32)=[N:3]1.C(N(CC)CC)C.[C:24](OC(=O)C)(=[O:26])[CH3:25]>O1CCCC1.C(=O)([O-])O.[Na+].C(OCC)(=O)C>[CH3:1][N:2]1[CH:10]=[C:9]2[C:4]([CH:5]=[CH:6][C:7]3[CH2:13][CH2:12][C:11](=[CH:14][CH2:15][NH:16][C:24](=[O:26])[CH3:25])[C:8]=32)=[N:3]1

参加物

7

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 686989692-(2-methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethanamine

生成物 1

HCID 68700363N-[2-(2-methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethyl]acetamide収率 82%

試薬・触媒・溶媒 3

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

2-(2-Methyl-6,7-dihydrocyclopenta[e]indazol-8(2H)-ylidene)ethanamine (400 mg, 1.88 mmol) was dissolved in tetrahydrofuran (19 mL), triethylamine (287 μL, 2.06 mmol) and acetic anhydride (195 μL, 2.06 mmol) were added under ice-cooling, and the mixture was stirred for 15 min. The reaction solution was diluted with saturated aqueous sodium hydrogen carbonate solution, diluted with ethyl acetate, washed with water and saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→10/90) to give the title compound (393 mg, yield 82%).

後処理

  1. temperaturecooling
  2. washwashed with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (methanol/ethyl acetate=0/100→10/90)

出典と根拠

ORDレコード
ord-805bbc0badea412ba49fc5ee5984fb2d
出典データセット
uspto-grants-2012_08
特許番号
US08247429B2

関連ノート

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