Hydrochloride methanol → HCID 21993796, compound

HRID 1978479Notes

Reaction equation

HRID 1978479 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([CH2:16][NH:17][C:18]([CH: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)[CH2:21]3)=[O:19])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:32].CO>C(O)C>[ClH:32].[ClH:32].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH:13]([CH2:16][NH:17][C:18]([CH: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)[CH2:21]3)=[O:19])[CH2:14][CH2:15]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993797HCID 21993797, compound

Product 1

HCID 21993796HCID 21993796, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 583.9 mg (1.34 mM) of N-[1-(3-phenylpropan-1-yl)piperidin-4-ylmethyl]-3,4-dihydro-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (5 ml) was added 10 ml (40 mM) of 4N-HCl/methanol and the mixture was stirred at room temperature for several minutes. After the solvent was distilled off under reduced pressure, 2-propanol was added and the resulting crystals were filtered off. The filtrate was concentrated to provide the title compound as light-brown amorphous substance.

Workup

  1. distillationAfter the solvent was distilled off under reduced pressure, 2-propanol
  2. additionwas added
  3. filtrationthe resulting crystals were filtered off
  4. concentrationThe filtrate was concentrated

Sources & evidence

ORD record
ord-5791422a2e4243dea0324c6fb345d6ac
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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