Hydrochloride methanol → HCID 21993742, compound

HRID 1978424Notes

Reaction equation

HRID 1978424 reaction equation
[C:1]1([CH:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18]([C:20]3[S:30][C:29]4[N:31]5[C:22](=[CH:23][N:24]=[C:25]5[CH:26]=[CH:27][CH:28]=4)[CH:21]=3)=[O:19])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:32].CO>C(O)C>[ClH:32].[ClH:32].[C:1]1([CH:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18]([C:20]3[S:30][C:29]4[N:31]5[C:22](=[CH:23][N:24]=[C:25]5[CH:26]=[CH:27][CH:28]=4)[CH:21]=3)=[O:19])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993743HCID 21993743, compound

Product 1

HCID 21993742HCID 21993742, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.76 g (4.07 mM) of N-[4-(4-phenylpiperidin-1-yl)butan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (15 ml) was added 6 ml (24 mM) of 4N-HCl/methanol at room temperature and the mixture was stirred at the same temperature for several minutes. The solvent was then distilled off under reduced pressure and diethyl ether was added to the residue. The resulting crystals were collected by filtration and rinsed with diethyl ether to provide the title compound as orange-colored crystals.

Workup

  1. distillationThe solvent was then distilled off under reduced pressure and diethyl ether
  2. additionwas added to the residue
  3. filtrationThe resulting crystals were collected by filtration
  4. washrinsed with diethyl ether

Sources & evidence

ORD record
ord-228a5e35df3e484d8a9f28707c768b8d
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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