Ethyl Acetate → HCID 67333040, 화합물

HRID 1886962노트

반응식

HRID 1886962 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 67333040HCID 67333040, 화합물수율 48%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-5a589535934440bb8b5a494fea631b53
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501713B2

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