Potassium Acetate → 5H,6H,7H,8H,9H-pyrido(3,2-b)azepin-6-one
반응식
CC1C=CC(S(O[N:12]=[C:13]2[CH2:22][CH2:21][CH2:20][C:19]3[N:18]=[CH:17][CH:16]=[CH:15][C:14]2=3)(=O)=O)=CC=1.C([O-])(=[O:25])C.[K+]>CCO.O>[N:18]1[C:19]2[CH2:20][CH2:21][CH2:22][C:13](=[O:25])[NH:12][C:14]=2[CH:15]=[CH:16][CH:17]=1참가 물질
5
실험 절차
A mixture of 1.0 eq of 95 and 2.3 eq of potassium acetate in 70 mL of EtOH and 140 mL of H2O was refluxed for 17 hrs. After cooling to rt and rotary evaporation of the EtOH, the solution was made alkaline with 10 N NaOH. The mixture was extracted with chloroform (3×50 mL). The combined organic extracts were dried over MgSO4 and vacuum filtered. The filtrate was rotary evaporated and dried under vacuum to yield 96.
후처리
- temperaturewas refluxed for 17 hrs
- customrotary evaporation of the EtOH
- extractionThe mixture was extracted with chloroform (3×50 mL)
- dry with materialThe combined organic extracts were dried over MgSO4 and vacuum
- filtrationfiltered
- customThe filtrate was rotary evaporated
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-1274ecf09d6440cdb06d900122c2621f
- 출처 데이터셋
- uspto-grants-2008_08
- 특허 번호
- US07417152B2
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