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[CH2:1]([N:3]([CH2:26][CH3:27])[S:4]([C:7]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:10]2[N:11]=C(C3C=CC=CC=3)[O:13][C:9]=2[CH:8]=1)(=[O:6])=[O:5])[CH3:2].[OH-].[K+]>C(O)C>[CH2:26]([N:3]([CH2:1][CH3:2])[S:4]([C:7]1[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[C:10]([NH2:11])=[C:9]([OH:13])[CH:8]=1)(=[O:6])=[O:5])[CH3:27]참가 물질
4
실험 절차
A mixture of N,N-diethyl-2-phenylnaphth[1,2-d]oxazole-5-sulfonamide (38.1 g, 100 mmol), 20% KOH (140 ml) and ethanol (180 ml) was refluxed for 24 h under nitrogen and the product was extracted with ethyl acetate (3×500 ml). The combined extracts were dried over anhydrous sodium sulfate and the solvent evaporated to give 45.4 g crude N,N-diethyl-4-amino-3-hydroxy-1-naphthalenesulfonamide as a black sticky oil (50% pure by NMR). An analytical sample was prepared by column chromatography (chloroform) to give pure N,N-diethyl-4-amino-3-hydroxy-1-naphthalenesulfonamide as a glassy material which upon trituration with ether gave a black solid, m.p. 120°-122° C.
후처리
- temperaturewas refluxed for 24 h under nitrogen
- extractionthe product was extracted with ethyl acetate (3×500 ml)
- dry with materialThe combined extracts were dried over anhydrous sodium sulfate
- customthe solvent evaporated
출처 및 근거
- ORD 기록
- ord-029b2ddab4604ea28c30360825584374
- 출처 데이터셋
- uspto-grants-1994_05
- 특허 번호
- US05314998
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