Methyl iodide → HCID 21447150, compound

HRID 1415512Notes

Reaction equation

HRID 1415512 reaction equation
[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]

Participants

3

Reactant 2

HCID 6328Methyl iodideHCID 1207378757415-52-8

Product 1

HCID 21447150HCID 21447150, compound

Procedure

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 mixtures is extracted with methanol, and the methanol extracts are concentrated to provide a crystalline solid wich 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(2,2,2trifluoroethoxy)benzamidomethyl]-1,1-dimethylpiperidinium iodide, m.p. 170° -172.5° C.

Workup

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

Sources & evidence

ORD record
ord-8a8b14c3e07e4995bf8f70c369a9dd6f
Source dataset
uspto-grants-1977_01
Patent number
US04005209

Reaction notes

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