Methyl iodide → HCID 18472580, compound

HRID 565931Notes

Reaction equation

HRID 565931 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][CH:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH2:15][C:14]([C:24]([NH:26][C:27]4[CH:32]=[CH:31][C:30]([CH2:33][N:34]5[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]5)=[CH:29][CH:28]=4)=[O:25])=[CH:13][C:12]=3[CH:40]=2)=[CH:4][CH:3]=1.[CH3:41][I:42]>CN(C)C=O>[I-:42].[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH:16]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH2:15][C:14]([C:24]([NH:26][C:27]4[CH:28]=[CH:29][C:30]([CH2:33][N+:34]5([CH3:41])[CH2:35][CH2:36][CH2:37][CH2:38][CH2:39]5)=[CH:31][CH:32]=4)=[O:25])=[CH:13][C:12]=3[CH:40]=2)=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 6328Methyl iodideHCID 18472507HCID 18472507, compound

Product 1

HCID 18472580HCID 18472580, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

A solution of 7-(4-methylphenyl)-2-phenyl-N-(4-(piperidinomethyl)-phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (0.08g) and methyl iodide (0.05ml) in dimethylformamide (15ml) 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-phenyl-2,3-dihydro-1-benzoxepin-4-carbonyl)-4-aminobenzyl)-1-methyl-piperidinium iodide (Compound 103) (0.057g) 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-59e5fd8cd89948f6a78a6142dcf87c79
Source dataset
uspto-grants-2001_01
Patent number
US06172061B2

Reaction notes

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