Hydrochloride methanol → HCID 21993693, compound

HRID 1978451Notes

Reaction equation

HRID 1978451 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:14][CH2:13][CH:12]([NH:15][C:16]([C:18]3[S:28][C:27]4[N:29]5[C:20](=[CH:21][N:22]=[C:23]5[CH:24]=[CH:25][CH:26]=4)[CH:19]=3)=[O:17])[CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:30].CO>C(O)C>[ClH:30].[ClH:30].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:14][CH2:13][CH:12]([NH:15][C:16]([C:18]3[S:28][C:27]4[N:29]5[C:20](=[CH:21][N:22]=[C:23]5[CH:24]=[CH:25][CH:26]=4)[CH:19]=3)=[O:17])[CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993694HCID 21993694, compound

Product 1

HCID 21993693HCID 21993693, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 242.4 mg (0.60 mM) of N-[1-(3-phenylpropan-1-yl)pyrrolidin-3-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (2 ml) was added 1.5 ml (6.0 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 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 diethyl ether

Sources & evidence

ORD record
ord-d19dfd7cbfc84d79b1e371d3eb07d4be
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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