Methyl iodide → 2-[4-(5-Carbamoyloxymethyl-isoxazol-3-yl)-phenoxymethyl]-1-methyl-pyridinium iodide
반응식
[I:1][CH3:2].[N:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:21]=[C:20]([CH2:22][O:23][C:24](=[O:26])[NH2:25])[O:19][N:18]=2)=[CH:13][CH:12]=1>>[I-:1].[C:24]([O:23][CH2:22][C:20]1[O:19][N:18]=[C:17]([C:14]2[CH:13]=[CH:12][C:11]([O:10][CH2:9][C:4]3[CH:5]=[CH:6][CH:7]=[CH:8][N+:3]=3[CH3:2])=[CH:16][CH:15]=2)[CH:21]=1)(=[O:26])[NH2:25]참가 물질
3
반응 조건
- 온도
- 80 °C
실험 절차
2 ml of iodomethane was added to 0.3 g of the compound carbamic acid 3-[4-(pyridin-2-ylmethoxy)-phenyl]-isoxazol-5-ylmethyl ester in Example 65 and stirred at 80° C. for 10 hours. A crude solid compound obtained after distillation of the solution under reduced pressure to remove an excess of MeI was recrystallized from ethyl acetate/hexane/methylene chloride to obtain 2-[4-(5-carbamoyloxymethyl-isoxazol-3-yl)-phenoxymethyl]-1-methyl-pyridinium iodide as a desired compound.
후처리
- customA crude solid compound obtained
- distillationafter distillation of the solution under reduced pressure
- customto remove an excess of MeI
- customwas recrystallized from ethyl acetate/hexane/methylene chloride
출처 및 근거
- ORD 기록
- ord-e34c5829394a4b9ea6b994b276744f62
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08828992B2
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