Methyl iodide → HCID 18472580, compound

HRID 2228126Notes

Reaction equation

HRID 2228126 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. 08 g) and methyl iodide (0.05 ml) in dimethylformamide (15 ml) was stirred at room temperature overnight. 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-methylpiperidinium iodide (Compound 103) (0.057 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-6d288f988a1b45588ca0dedad4a01d4a
Source dataset
uspto-grants-2002_07
Patent number
US06413947B1

Reaction notes

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