Hydrochloride methanol → HCID 21993747, compound

HRID 1978426Notes

Reaction equation

HRID 1978426 reaction equation
[CH2:1]([CH:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][CH2:17][NH:18][C:19]([C:21]2[S:31][C:30]3[N:32]4[C:23](=[CH:24][N:25]=[C:26]4[CH:27]=[CH:28][CH:29]=3)[CH:22]=2)=[O:20])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:33].CO>C(O)C>[ClH:33].[ClH:33].[CH2:1]([CH:8]1[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][CH2:17][NH:18][C:19]([C:21]2[S:31][C:30]3[N:32]4[C:23](=[CH:24][N:25]=[C:26]4[CH:27]=[CH:28][CH:29]=3)[CH:22]=2)=[O:20])[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 21993660HCID 21993660, compound

Product 1

HCID 21993747HCID 21993747, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 2.00 g (4.48 mM) of N-[4-(4-benzylpiperidin-1-yl)butan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (20 ml) was added 10 ml (40 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, diethyl ether was added to the residue and the mixture was cooled to 0° C. The resulting crystals were collected 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, diethyl ether
  2. additionwas added to the residue
  3. temperaturethe mixture was cooled to 0° C
  4. filtrationThe resulting crystals were collected by filtration
  5. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-c861549797ff4b908d11dbd95d8d8a47
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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