Water → ethyl 4H-thieno[3,2-b]pyrrole-5-carboxylate
반응식
[CH2:1]([O:3][C:4](=[O:15])[C:5]([N:12]=[N+]=[N-])=[CH:6][C:7]1[S:8][CH:9]=[CH:10][CH:11]=1)[CH3:2].O>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4]([C:5]1[NH:12][C:11]2[CH:10]=[CH:9][S:8][C:7]=2[CH:6]=1)=[O:15])[CH3:2]참가 물질
4
실험 절차
The resulting azide, 2-azido-3-thiophen-2-yl-acrylic acid ethyl ester (650 mg, 2.88 mmol) was dissolved in toluene (40 ml) and the solution was refluxed for 2 hours. The solution was thereafter cooled, and water (80 ml) was added. After separation of the phases the aqueous phase was extracted with ethyl acetate (3×20 ml), the combined organic phase was dried over Na2SO4 and the organic solvents were evaporated under reduced pressure. The crude product was purified by silica gel flash chromatography to give 450 mg of pure 4H-thieno[3,2-b]pyrrole-5-carboxylic acid ethyl ester (80% yield).
후처리
- temperaturethe solution was refluxed for 2 hours
- temperatureThe solution was thereafter cooled
- customAfter separation of the phases the aqueous phase
- extractionwas extracted with ethyl acetate (3×20 ml)
- dry with materialthe combined organic phase was dried over Na2SO4
- customthe organic solvents were evaporated under reduced pressure
- customThe crude product was purified by silica gel flash chromatography
출처 및 근거
- ORD 기록
- ord-5ec4183f2c9342808eaca87fe02f2cba
- 출처 데이터셋
- uspto-grants-2010_09
- 특허 번호
- US07795255B2
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