Hydrochloride methanol → HCID 21993848, compound

HRID 1978440Notes

Reaction equation

HRID 1978440 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH2:16][CH2:17][CH2:18][NH:19][C:20]([C:22]3[S:32][C:31]4[N:33]5[C:24](=[CH:25][N:26]=[C:27]5[CH:28]=[CH:29][CH:30]=4)[CH:23]=3)=[O:21])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:34].CO>C(O)C>[ClH:34].[ClH:34].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH:13]([CH2:16][CH2:17][CH2:18][NH:19][C:20]([C:22]3[S:32][C:31]4[N:33]5[C:24](=[CH:25][N:26]=[C:27]5[CH:28]=[CH:29][CH:30]=4)[CH:23]=3)=[O:21])[CH2:14][CH2:15]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993849HCID 21993849, compound

Product 1

HCID 21993848HCID 21993848, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 0.8113 g (1.76 mM) of N-[3-(1-(3-phenylpropan-1-yl)piperidin-4-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. The solvent was then distilled off under reduced pressure, and after addition of diethyl ether to the crystalline residue, the crystal crop was harvested by filtration and rinsed with ethanol and diethyl ether to provide the title compound.

Workup

  1. distillationThe solvent was then distilled off under reduced pressure
  2. additionafter addition of diethyl ether to the crystalline residue
  3. filtrationthe crystal crop was harvested by filtration
  4. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-d9cdbf5b3cac4c45b80ff86a2d20c250
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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