Hydrochloride methanol → HCID 21994102, compound

HRID 1978449Notes

Reaction equation

HRID 1978449 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][NH:18][C:19]([C:21]3[S:31][C:30]4[N:32]5[C:23](=[CH:24][N:25]=[C:26]5[CH:27]=[CH:28][CH:29]=4)[CH:22]=3)=[O:20])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:33].CO>C(O)C>[ClH:33].[ClH:33].[ClH:33].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([CH2:16][CH2:17][NH:18][C:19]([C:21]3[S:31][C:30]4[N:32]5[C:23](=[CH:24][N:25]=[C:26]5[CH:27]=[CH:28][CH:29]=4)[CH:22]=3)=[O:20])[CH2:14][CH2:15]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993602HCID 21993602, compound

Product 1

HCID 21994102HCID 21994102, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.15 g (2.57 mM) of N-[2-(4-(3-phenylpropan-1-yl)piperazin-1-yl)ethan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added 4 ml (16 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 diethyl ether was added to the residue. The resulting crystals were collected 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 and diethyl ether
  2. additionwas added to the residue
  3. filtrationThe resulting crystals were collected by filtration
  4. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-ec3799fc2bad4713944150859c1f962c
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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