Hydrochloride methanol → N-[1-(4-phenoxybutan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Dihydrochloride

HRID 1978466Notes

Reaction equation

HRID 1978466 reaction equation
[O:1]([CH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH2:17][CH2:16][CH:15]([CH2:18][NH:19][C:20]([C:22]2[S:32][C:31]3[N:33]4[C:24](=[CH:25][N:26]=[C:27]4[CH:28]=[CH:29][CH:30]=3)[CH:23]=2)=[O:21])[CH2:14][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:34].CO>C(O)C>[ClH:34].[ClH:34].[O:1]([CH2:8][CH2:9][CH2:10][CH2:11][N:12]1[CH2:17][CH2:16][CH:15]([CH2:18][NH:19][C:20]([C:22]2[S:32][C:31]3[N:33]4[C:24](=[CH:25][N:26]=[C:27]4[CH:28]=[CH:29][CH:30]=3)[CH:23]=2)=[O:21])[CH2:14][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993919N-[1-(4-phenoxybutan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide

Product 1

HCID 21994002N-[1-(4-phenoxybutan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Dihydrochloride

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 0.3241 g (0.70 mM) of N-[1-(4-phenoxybutan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (4 ml) was added 1.0 ml (4 mM) of 4N-HCl/methanol. The solvent was distilled off under reduced pressure and the residue was diluted with ethanol and ether. 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
  2. additionthe residue was diluted with ethanol and ether
  3. filtrationThe resulting crystals were collected by filtration
  4. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-97f89d54616d41d0a13c0b984f1846ea
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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