Hydrochloride methanol → HCID 21994016, compound

HRID 1978430Notes

Reaction equation

HRID 1978430 reaction equation
[C:1]1([N:7]2[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18]([C:20]3[S:30][C:29]4[N:31]5[C:22](=[CH:23][N:24]=[C:25]5[CH:26]=[CH:27][CH:28]=4)[CH:21]=3)=[O:19])[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:32].CO>C(O)C>[ClH:32].[ClH:32].[ClH:32].[C:1]1([N:7]2[CH2:8][CH2:9][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18]([C:20]3[S:30][C:29]4[N:31]5[C:22](=[CH:23][N:24]=[C:25]5[CH:26]=[CH:27][CH:28]=4)[CH:21]=3)=[O:19])[CH2:11][CH2:12]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21994017HCID 21994017, compound

Product 1

HCID 21994016HCID 21994016, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.37 g (3.16 mM) of N-[4-(4-phenyl-1-piperazinyl)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 3 hours (crystals separated out). 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. custom(crystals separated out)
  2. distillationAfter the solvent was distilled off under reduced pressure, ethanol and diethyl ether
  3. additionwere added to the residue
  4. filtrationthe resulting crystals were collected by filtration
  5. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-050b2f8a89ee495fbbf41ecd06533d2b
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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