Methyl iodide → HCID 9938497, compound

HRID 2228123Notes

Reaction equation

HRID 2228123 reaction equation
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:26]=[CH:25][C:24]([CH2:27][N:28]5[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]5)=[CH:23][CH:22]=4)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:4][CH:3]=1.[CH3:35][I:36]>CN(C)C=O>[I-:36].[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:22]=[CH:23][C:24]([CH2:27][N+:28]5([CH3:35])[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]5)=[CH:25][CH:26]=4)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 6328Methyl iodideHCID 3013432HCID 3013432, compound

Product 1

HCID 9938497HCID 9938497, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

A solution of 7—(4-methylphenyl)-N-(4—(piperidinomethyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (1.4 g) and methyl iodide (0.58 ml) in dimethylformamide (50 ml) was stirred at room temperature over night. The solvent was evaporated, and to the residue was added ethyl acetate. Precipitated crude crystal was filtered, which were recrystallized from ethanol-ethyl acetate to give 1—(N-(7—(4-methylphenyl)-2,3-dihydro-1-benzoxepin-4-carbonyl)-4-aminobenzyl)-1-methylpiperidinium iodide (Compound 96) (1.6 g) as colorless crystals.

Workup

  1. customThe solvent was evaporated
  2. additionto the residue was added ethyl acetate
  3. customPrecipitated crude crystal
  4. filtrationwas filtered
  5. customwhich were recrystallized from ethanol-ethyl acetate

Sources & evidence

ORD record
ord-5b2ea8ba2f9c4df591173434bef49b76
Source dataset
uspto-grants-2002_07
Patent number
US06413947B1

Reaction notes

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