Ethyl Acetate → HCID 67333040、化合物

HRID 1886962ノート

反応式

HRID 1886962 の反応式
[C:1]1([C:7]2[O:8][C:9]3[CH:15]=[CH:14][C:13]([NH2:16])=[CH:12][C:10]=3[CH:11]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:17](Cl)(=[O:21])[CH:18]([CH3:20])[CH3:19].C(OCC)(=O)C>N1C=CC=CC=1>[C:1]1([C:7]2[O:8][C:9]3[CH:15]=[CH:14][C:13]([NH:16][C:17](=[O:21])[CH:18]([CH3:20])[CH3:19])=[CH:12][C:10]=3[CH:11]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 62325Isobutyryl chlorideHCID 167651722-Phenyl-1-benzofuran-5-amine

生成物 1

HCID 67333040HCID 67333040、化合物収率 48%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 2-phenylbenzofuran-5-amine (210 mg, 1.00 mmol) in pyridine (5 mL) at room temperature was added isobutyryl chloride (120 μL, 1.10 mmol). The resulting mixture was stirred at room temperature for 16 h. Ethyl acetate was added and the organic layer was washed with saturated aqueous copper sulfate solution followed by saturated aqueous potassium carbonate solution. The combined organic layers were dried over anhydrous MgSO4 and evaporated. The resulting material was purified by column chromatography eluting using a gradient (ethyl acetate/hexanes 1:3 v/v to ethyl acetate/hexanes 1:2 v/v) to afford 134 mg (48%) of the title compound (LCMS RT=6.81 min, MH+ 280.1)

後処理

  1. washthe organic layer was washed with saturated aqueous copper sulfate solution
  2. dry with materialThe combined organic layers were dried over anhydrous MgSO4
  3. customevaporated
  4. customThe resulting material was purified by column chromatography
  5. washeluting

出典と根拠

ORDレコード
ord-5a589535934440bb8b5a494fea631b53
出典データセット
uspto-grants-2013_08
特許番号
US08501713B2

反応ノート

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