HCID 9811366, compound → HCID 21994031, compound

HRID 1978433Notes

Reaction equation

HRID 1978433 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][CH:13]([NH:16][C:17]([C:19]3[S:29][C:28]4[N:30]5[C:21](=[CH:22][N:23]=[C:24]5[CH:25]=[CH:26][CH:27]=4)[CH:20]=3)=[O:18])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:31].CO>C(O)C>[ClH:31].[ClH:31].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][CH:13]([NH:16][C:17]([C:19]3[S:29][C:28]4[N:30]5[C:21](=[CH:22][N:23]=[C:24]5[CH:25]=[CH:26][CH:27]=4)[CH:20]=3)=[O:18])[CH2:14][CH2:15]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 2

HCID 9811366HCID 9811366, compoundHCID 21893726Hydrochloride methanol

Product 1

HCID 21994031HCID 21994031, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 356.2 mg (0.85 mM) of N-[1-(3-phenylpropan-1-yl)piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (6 ml) was added 2.0 ml (8.0 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 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, 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-0269f3f977154fcf92bf0970243340cd
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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