Dimethylformamide → HCID 18472428, compound

HRID 1277103Notes

Reaction equation

HRID 1277103 reaction equation
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[S:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:26]=[CH:25][C:24](N5CCCCC5)=[CH:23][C:22]=4C)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:4][CH:3]=1.C[I:36].[CH3:37][N:38]([CH3:41])[CH:39]=O>>[I-:36].[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[S:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:26]=[CH:25][C:24]([CH2:37][N+:38]5([CH3:41])[CH2:4][CH2:3][CH2:2][CH2:1][CH2:39]5)=[CH:23][CH:22]=4)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:6][CH:7]=1

Participants

4

Reactant 3

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 69352297HCID 69352297, compound

Product 1

HCID 18472428HCID 18472428, compound

Procedure

A solution of 7-(4-methylphenyl)-N-(4-piperidino-methyl-phenyl)-2,3-dihydro-1-benzothiepine-4-carboxamide (0.08 g) and methyl iodide (0.013 ml) in dimethylformamide (20 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-hexane to give 1-(N-(7-(4-methylphenyl)-2,3-dihydro-1-benzothiepine-4-carbonyl)-4-aminobenzyl)-1-methylpiperidinium iodide (Compound 94) (0.077 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-hexane

Sources & evidence

ORD record
ord-0181bf05e4e949a4bc56c70408f04941
Source dataset
uspto-grants-2000_12
Patent number
US06166006

Reaction notes

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