Methyl iodide → HCID 21715701, compound

HRID 1277149Notes

Reaction equation

HRID 1277149 reaction equation
[N:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:14]=[CH:15][C:16]4[O:22][CH2:21][CH2:20][C:19]([C:23]([NH:25][C:26]5[CH:31]=[CH:30][C:29]([CH2:32][N:33]([CH:35]6[CH2:40][CH2:39][O:38][CH2:37][CH2:36]6)[CH3:34])=[CH:28][CH:27]=5)=[O:24])=[CH:18][C:17]=4[CH:41]=3)=[CH:9][CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:42][I:43]>CN(C)C=O>[I-:43].[CH3:34][N+:33]([CH3:42])([CH2:32][C:29]1[CH:30]=[CH:31][C:26]([NH:25][C:23]([C:19]2[CH2:20][CH2:21][O:22][C:16]3[CH:15]=[CH:14][C:13]([C:10]4[CH:9]=[CH:8][C:7]([N:1]5[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]5)=[CH:12][CH:11]=4)=[CH:41][C:17]=3[CH:18]=2)=[O:24])=[CH:27][CH:28]=1)[CH:35]1[CH2:36][CH2:37][O:38][CH2:39][CH2:40]1

Participants

4

Reactant 2

HCID 6328Methyl iodideHCID 18472465HCID 18472465, compound

Product 1

HCID 21715701HCID 21715701, compound

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

A solution of 7-(4-piperidinophenyl)-N-(4-((N-tetrahydropyran-4-yl-N-methylamino)methyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (0.2 g) and methyl iodide (0.025 ml) in dimethylformamide (5 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 dimethyl(N-(7-(4-piperidinophenyl)-2,3-dihydro-1-benzoxepin-4-carbonyl)-4-aminobenzyl)-4-tetrahydropyranylammonium iodide (Compound 221) (0.1 g) as yellow 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-147a5f6e600049fb9eee47f661c5d9fa
Source dataset
uspto-grants-2000_12
Patent number
US06166006

Reaction notes

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