Hydrochloride methanol → HCID 21993952, compound

HRID 1978428Notes

Reaction equation

HRID 1978428 reaction equation
[CH2:1]([CH:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][NH:17][C:18]([C:20]2[S:30][C:29]3[N:31]4[C:22](=[CH:23][N:24]=[C:25]4[CH:26]=[CH:27][CH:28]=3)[CH:21]=2)=[O:19])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:32].CO>C(O)C>[ClH:32].[ClH:32].[CH2:1]([CH:8]1[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][NH:17][C:18]([C:20]2[S:30][C:29]3[N:31]4[C:22](=[CH:23][N:24]=[C:25]4[CH:26]=[CH:27][CH:28]=3)[CH:21]=2)=[O:19])[CH2:12][CH2:13]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993953HCID 21993953, compound

Product 1

HCID 21993952HCID 21993952, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.84 g (4.25 mM) of N-[3-(4-benzylpiperidin-1-yl)propan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added 6 ml (24 mM) of 4N-HCl/methanol at room temperature and the mixture was stirred at room temperature for several minutes. After the solvent was distilled off under reduced pressure, ethanol and diethyl ether were added to the crystalline residue. The crystal crop was then harvested by filtration and rinsed with ethanol and diethyl ether to provide the title compound as orange-colored crystals.

Workup

  1. distillationAfter the solvent was distilled off under reduced pressure, ethanol and diethyl ether
  2. additionwere added to the crystalline residue
  3. filtrationThe crystal crop was then harvested by filtration
  4. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-a9d7320771654511acfe7fddb8a9cdf6
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

Loading…