Hydrochloride methanol → HCID 21993934, compound

HRID 1978436Notes

Reaction equation

HRID 1978436 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH2:16][CH2:17][NH:18][C:19]([C:21]3[S:31][C:30]4[N:32]5[C:23](=[CH:24][N:25]=[C:26]5[CH:27]=[CH:28][CH:29]=4)[CH:22]=3)=[O:20])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:33].CO>C(O)C>[ClH:33].[ClH:33].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH:13]([CH2:16][CH2:17][NH:18][C:19]([C:21]3[S:31][C:30]4[N:32]5[C:23](=[CH:24][N:25]=[C:26]5[CH:27]=[CH:28][CH:29]=4)[CH:22]=3)=[O:20])[CH2:14][CH2:15]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993935HCID 21993935, compound

Product 1

HCID 21993934HCID 21993934, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 0.5142 g (1.15 mM) of N-[2-(1-(3-phenylpropan-1-yl)piperidin-4-yl)ethan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added 4 ml (16 mM) of 4N-HCl/methanol at room temperature and the mixture was stirred at room temperature for several minutes. The solvent was distilled off under reduced pressure and diethyl ether was added to the residue. The resulting crystals were collected by filtration and rinsed with ethanol and diethyl ether to provide the title compound.

Workup

  1. distillationThe solvent was 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 ethanol and diethyl ether

Sources & evidence

ORD record
ord-dd365665359e4ba4a5c19b6486527c8a
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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