HCID 22262599, compound → HCID 22262592, compound

HRID 489787Notes

Reaction equation

HRID 489787 reaction equation
[NH2:1][C:2]1[N:7]=[C:6]([O:8]C)[C:5]([C:10]([NH:12][CH2:13][CH:14]2[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][O:23][CH3:24])[CH2:16][CH2:15]2)=[O:11])=[CH:4][C:3]=1[Cl:25]>Cl>[NH2:1][C:2]1[NH:7][C:6](=[O:8])[C:5]([C:10]([NH:12][CH2:13][CH:14]2[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][O:23][CH3:24])[CH2:16][CH2:15]2)=[O:11])=[CH:4][C:3]=1[Cl:25]

Participants

3

Reactant 1

HCID 22262599HCID 22262599, compound

Product 1

HCID 22262592HCID 22262592, compoundYield 55.4%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent2×

Procedure

A solution of 6-amino-5-chloro-2-(methyloxy)-N-({1-[3-(methyloxy)propyl]-4-piperidinyl}methyl)-3-pyridinecarboxamide (step 3, 160 g, 0.43 mmol) in concentrated hydrochloric acid (2.5 ml) and 10% methanolic hydrochloric acid (10 ml) was stirred at 80° C. for 7 h. After cooling to room temperature, the solvent was removed in vacuo. The residue was suspended in diisopropyl ether and the precipitate was collected by filtration to give 85 mg (46%) of the title compound as a white amorphous solid.

Workup

  1. customthe solvent was removed in vacuo
  2. filtrationthe precipitate was collected by filtration

Sources & evidence

ORD record
ord-8a71697f9edf464e88b8badac7500c19
Source dataset
uspto-grants-2005_12
Patent number
US06979690B2

Reaction notes

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