Hydrochloride methanol → N-[1-(3-(2-fluorophenyl)propan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Dihydrochloride

HRID 1978457Notes

Reaction equation

HRID 1978457 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([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])[CH2:13][CH2:12]1.[ClH:33].CO>C(O)C>[ClH:33].[ClH:33].[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([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])[CH2:13][CH2:12]1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993941N-[1-(3-(2-fluorophenyl)propan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide

Product 1

HCID 21994097N-[1-(3-(2-fluorophenyl)propan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Dihydrochloride

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 347 mg (0.8 mM) of N-[1-(3-(2-fluorophenyl)propan-1-yl)piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (4 ml) was added 1.0 ml (4.0 mM) of 4N-HCl/methanol. After the solvent was distilled off under reduced pressure, ethanol and diethyl ether were added to the residue and the resulting crystals were collected by filtration and rinsed with ethanol and diethyl ether to provide the title compound.

Workup

  1. distillationAfter the solvent was distilled off under reduced pressure, ethanol and diethyl ether
  2. additionwere added to the residue
  3. filtrationthe resulting crystals were collected by filtration
  4. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-1b4ffb7de5bf4df081f410abd8291444
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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