반응식
[Na].[NH2:2][C:3]1[C:7]([CH3:8])=[CH:6][S:5][C:4]=1C(O)=O.[CH3:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:19]2Cl.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.C(O)(=O)C>[CH3:12][O:13][C:14]1[CH:15]=[CH:16][CH:17]=[C:18]2[C:23]=1[N:22]=[CH:21][C:20]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[C:19]2[NH:2][C:3]1[C:7]([CH3:8])=[CH:6][S:5][CH:4]=1참가 물질
8
실험 절차
The sodium salt of 3-amino-4-methylthiophene-2-carboxylic acid (7.2 g, 0.04 mol) and ethyl 8-methoxy-4-chloroquinoline-3-carboxylate (5.39 g, 0.02 mol) in toluene (75 ml), ethanol (55 ml) and glacial acetic acid (10 ml) were stirred at room temperature for five days. The solvents were removed by evaporation at reduced pressure to give a dark-green slurry. 10% aqueous sodium carbonate was added and the insoluble solid filtered off, washed well with water and dried. This material was crystallised from ethyl acetate (with charcoaling) to give the title compound as pale yellow crystals (2.15 g), m.p. 162°-164°.
후처리
- customThe solvents were removed by evaporation at reduced pressure
- customto give a dark-green slurry
- filtrationthe insoluble solid filtered off
- washwashed well with water
- customdried
- customThis material was crystallised from ethyl acetate (with charcoaling)
출처 및 근거
- ORD 기록
- ord-87d67d2a1bf3431799652c6e30b4cd43
- 출처 데이터셋
- uspto-grants-1991_04
- 특허 번호
- US05006535
연결된 노트
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