Ethanol → HCID 18668782, compound

HRID 1058630Notes

Reaction equation

HRID 1058630 reaction equation
[Cl:1][C:2]1[C:11]2[N:12]=[C:13]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[N:14]([CH2:15][CH2:16][N:17]3[CH2:22][CH2:21][N:20](C(OC(C)(C)C)=O)[CH2:19][CH2:18]3)[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1.C(O)(C)C.C(O)C.[CH3:43][S:44]([OH:47])(=[O:46])=[O:45]>ClCCCl>[CH3:43][S:44]([OH:47])(=[O:46])=[O:45].[Cl:1][C:2]1[C:11]2[N:12]=[C:13]([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[N:14]([CH2:15][CH2:16][N:17]3[CH2:18][CH2:19][NH:20][CH2:21][CH2:22]3)[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1

Participants

6

Reactant 4

HCID 702EthanolHCID 3776IsopropanolHCID 6395Methanesulfonic AcidHCID 18668755HCID 18668755, compound

Product 1

HCID 18668782HCID 18668782, compound

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent

Procedure

To a solution of 1.20 g of tert-butyl 4-[2-(4-chloro-2-phenyl-1H-imidazo-[4,5-c]quinolin-1-yl)ethyl]-1-piperazinecarboxylate in 12 ml of 1,2-dichloroethane, 1.2 ml of methanesulfonic acid was added, and the mixture was stirred at room temperature for 5 minutes. The reaction mixture was added with isopropanol and ethanol, and the precipitated crystals were collected by filtration to give 1.24 g of colorless crystals. Recrystallization from methanol gave colorless crystals having the melting point of from 256 to 270° C. (decomposition).

Workup

  1. filtrationthe precipitated crystals were collected by filtration

Sources & evidence

ORD record
ord-e12102b6c5524660bce336a2d9a8b11e
Source dataset
uspto-grants-2003_02
Patent number
US06518265B1

Reaction notes

Loading…