Methyl iodide → HCID 21447150, 화합물

HRID 597225노트

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HRID 597225 반응식
[F:1][C:2]([F:29])([F:28])[CH2:3][O:4][C:5]1[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]([F:27])([F:26])[F:25])=[CH:18][C:6]=1[C:7]([NH:9][CH2:10][CH:11]1[CH2:16][CH2:15][CH2:14][CH2:13][N:12]1[CH3:17])=[O:8].[CH3:30][I:31]>>[I-:31].[F:29][C:2]([F:1])([F:28])[CH2:3][O:4][C:5]1[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]([F:27])([F:26])[F:25])=[CH:18][C:6]=1[C:7]([NH:9][CH2:10][CH:11]1[CH2:16][CH2:15][CH2:14][CH2:13][N+:12]1([CH3:30])[CH3:17])=[O:8]

참가 물질

3

실험 절차

A mixture of 2.7 g. (0.0063 mole) of finely divided 2.5-bis(2,2,2-trifluoroethoxy)-N-[(1-methyl-2-piperidyl)methyl]-benzamide and 6 ml. of methyl iodide is heated at 56° to 57° C. in a sealed tube for about 90 minutes. The mixture is extracted with methanol, and the methanol extracts are concentrated to provide a crystalline solid which is recrystallized from 50 ml. of ethyl acetate and about 2 ml. of isopropanol, with treatment by decolorizing charcoal. The resulting product is dried to provide white solid 2-[2,5-bis(2,2,2-trifluoroethoxy)benzamidomethyl]-1,1-dimethylpiperidinium iodide, m.p. 170°-172.5° C.

후처리

  1. additionA mixture of 2.7 g
  2. extractionThe mixture is extracted with methanol
  3. concentrationthe methanol extracts are concentrated
  4. customto provide a crystalline solid which
  5. customis recrystallized from 50 ml
  6. customThe resulting product is dried

출처 및 근거

ORD 기록
ord-3d2c98e4dd8440ae9bba4049ade7d4ba
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04013670

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