Sodium Carbonate → 2-Aminobenzimidazole
반응식
ClCCOCC.Br.Br.N1CCC([NH:15][C:16]2[NH:20][C:19]3[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=3[N:17]=2)CC1.C(=O)([O-])[O-].[Na+].[Na+].CN(C)C(=O)C>O>[NH:17]1[C:18]2[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=2[N:20]=[C:16]1[NH2:15]참가 물질
6
반응 조건
- 온도
- 70 °C
실험 절차
A mixture of 32 parts of 1-chloro-2-ethoxyethane, 94.5parts of N-(4-piperidinyl)-1H-benzimidazol-2-amine dihydrobromide, 90 parts of sodium carbonate and 540 parts of N,N-dimethylacetamide was stirred overnight at 70° C. After cooling, the reaction mixture was poured into water. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was boiled in acetonitrile. After cooling, the precipitated product was filtered off and dried, yielding 42.4 parts (58.8%) of N-[1-(2-ethoxyethyl)-4-piperidinyl[-1H-benzimidazol-2-amine; mp. 212° C. (interm. 29).
후처리
- temperatureAfter cooling
- extractionThe product was extracted with dichloromethane
- customThe extract was dried
- filtrationfiltered
- customevaporated
- temperatureAfter cooling
- filtrationthe precipitated product was filtered off
- customdried
출처 및 근거
- ORD 기록
- ord-a2dada330cdf4c488f3c7bb0c55e1fe3
- 출처 데이터셋
- uspto-grants-1990_07
- 특허 번호
- US04943580
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