Hydrochloric Acid → HCID 67662987, compound

HRID 2393301Notes

Reaction equation

HRID 2393301 reaction equation
C(OCC)(=O)C.[N:7]1([C:12]2[CH:13]=[CH:14][C:15]([O:51][CH3:52])=[C:16]([CH2:18][N:19]([CH2:46][CH2:47][CH2:48][CH2:49][CH3:50])[C:20]([NH:22][C:23]3[C:28]([CH3:29])=[CH:27][CH:26]=[CH:25][C:24]=3[O:30][CH2:31][CH2:32][CH2:33][N:34]3[CH2:39][CH2:38][N:37]([C:40]4[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=4)[CH2:36][CH2:35]3)=[O:21])[CH:17]=2)[CH:11]=[CH:10][N:9]=[CH:8]1.[ClH:53]>CCOCC>[ClH:53].[ClH:53].[ClH:53].[N:7]1([C:12]2[CH:13]=[CH:14][C:15]([O:51][CH3:52])=[C:16]([CH2:18][N:19]([CH2:46][CH2:47][CH2:48][CH2:49][CH3:50])[C:20]([NH:22][C:23]3[C:28]([CH3:29])=[CH:27][CH:26]=[CH:25][C:24]=3[O:30][CH2:31][CH2:32][CH2:33][N:34]3[CH2:35][CH2:36][N:37]([C:40]4[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=4)[CH2:38][CH2:39]3)=[O:21])[CH:17]=2)[CH:11]=[CH:10][N:9]=[CH:8]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 8857Ethyl Acetate2×HCID 9853086HCID 9853086, compound

Product 1

HCID 67662987HCID 67662987, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

Ethyl acetate (175 ml) was added to N-{5-(1-imidazolyl)-2-methoxyphenyl}methyl-N-(1-pentyl)-N'-[2-{3-(4-phenyl-1-piperazinyl)propoxy}-6-methylphenyl]urea (11.7 g, 0.0187 mol). The mixture was added dropwise with 4N HCl solution in ethyl acetate (16 ml, 0.064 mol) at room temperature with stirring. After stirred for 1 hour at room temperature, the mixture was added with ether (100 ml), and stirring was continued for 1 hour at room temperature. The precipitated amorphous crystals were collected by filtration under nitrogen atmosphere and dried at 60° C. under reduced pressure to give N-{5-(1-imidazolyl)-2-methoxyphenyl}methyl-N-(1-pentyl)-N'-[2-{3-(4-phenyl-1-piperazinyl)propoxy}-6-methyphenyl]urea trihydrochloride. (13.15 g).

Workup

  1. stirringAfter stirred for 1 hour at room temperature
  2. stirringstirring
  3. filtrationThe precipitated amorphous crystals were collected by filtration under nitrogen atmosphere
  4. customdried at 60° C. under reduced pressure

Sources & evidence

ORD record
ord-11cc4a4f701648f7b047bd09f709b3d4
Source dataset
uspto-grants-1998_09
Patent number
US05807860

Reaction notes

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