Hydrochloride methanol → HCID 21994198, compound

HRID 1978432Notes

Reaction equation

HRID 1978432 reaction equation
[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][N:2]1[CH2:11][CH2:12][CH2:13][CH2:14][NH:15][C:16]([C:18]1[S:28][C:27]2[N:29]3[C:20](=[CH:21][N:22]=[C:23]3[CH:24]=[CH:25][CH:26]=2)[CH:19]=1)=[O:17].[ClH:30].CO>C(O)C>[ClH:30].[ClH:30].[CH2:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:4][CH2:3][N:2]1[CH2:11][CH2:12][CH2:13][CH2:14][NH:15][C:16]([C:18]1[S:28][C:27]2[N:29]3[C:20](=[CH:21][N:22]=[C:23]3[CH:24]=[CH:25][CH:26]=2)[CH:19]=1)=[O:17]

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 21993811HCID 21993811, compound

Product 1

HCID 21994198HCID 21994198, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.76 g (4.35 mM) of N-[4-(1,2,3,4-tetrahydroisoquinolin-2-yl)butan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added 6 ml (24 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, ethanol was added to the residue and the mixture was concentrated. Then, diethyl ether was added and the crystal crop was harvested 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, ethanol
  2. additionwas added to the residue
  3. concentrationthe mixture was concentrated
  4. additionThen, diethyl ether was added
  5. filtrationthe crystal crop was harvested by filtration
  6. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-a118160fd5fd4c86a92ac0baa7298e9c
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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