Triethylamine → Methyl 4-(ethoxycarbonylamino)-thiophene-3-carboxylate
반응식
Cl.[NH2:2][C:3]1[C:4]([C:8]([O:10][CH3:11])=[O:9])=[CH:5][S:6][CH:7]=1.C(N(CC)CC)C.[C:19](Cl)(=[O:23])[O:20][CH2:21][CH3:22]>C1(C)C=CC=CC=1>[CH2:21]([O:20][C:19]([NH:2][C:3]1[C:4]([C:8]([O:10][CH3:11])=[O:9])=[CH:5][S:6][CH:7]=1)=[O:23])[CH3:22]참가 물질
5
실험 절차
A mixture of 50.0 g (0.258 mol) of methyl 4-aminothiophen-3-carboxylate-hydrochloride, 700 ml of toluene, 26 g (0.257 mol) of triethylamine and 27 ml (0.283 mol) of ethyl chlorocarbonate was refluxed for 5 hours. The insoluble matter was filtered off, the filtrate was evaporated down in vacuo and the residue was crystallised from petroleum ether. 59.0 g (99.8% of theory) of colourless crystals of melting point 52° C. were obtained.
후처리
- temperaturewas refluxed for 5 hours
- filtrationThe insoluble matter was filtered off
- customthe filtrate was evaporated down in vacuo
- customthe residue was crystallised from petroleum ether
- custom59.0 g (99.8% of theory) of colourless crystals of melting point 52° C. were obtained
출처 및 근거
- ORD 기록
- ord-ea670859d2e24feca0e7c78d11ba816f
- 출처 데이터셋
- uspto-grants-2002_02
- 특허 번호
- US06344449B1
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