Hydrochloric Acid → HCID 18770423, compound

HRID 1279452Notes

Reaction equation

HRID 1279452 reaction equation
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:14]2[CH:61]=[CH:60][C:17]([C:18]([N:20]3[CH2:25][CH2:24][N:23]([CH2:26][CH:27]4[CH2:32][CH2:31][CH:30]([CH2:33][N:34]5[CH2:39][CH2:38][N:37]([C:40](=[O:59])[C:41]6[CH:46]=[CH:45][C:44]([C:47]7[CH:52]=[C:51]([O:53][CH3:54])[C:50]([O:55][CH3:56])=[C:49]([O:57][CH3:58])[CH:48]=7)=[CH:43][CH:42]=6)[CH2:36][CH2:35]5)[CH2:29][CH2:28]4)[CH2:22][CH2:21]3)=[O:19])=[CH:16][CH:15]=2)[CH:7]=[C:8]([O:12][CH3:13])[C:9]=1[O:10][CH3:11]>C(O)C>[ClH:1].[ClH:1].[CH3:58][O:57][C:49]1[CH:48]=[C:47]([C:44]2[CH:45]=[CH:46][C:41]([C:40]([N:37]3[CH2:38][CH2:39][N:34]([CH2:33][CH:30]4[CH2:31][CH2:32][CH:27]([CH2:26][N:23]5[CH2:22][CH2:21][N:20]([C:18](=[O:19])[C:17]6[CH:60]=[CH:61][C:14]([C:6]7[CH:5]=[C:4]([O:3][CH3:2])[C:9]([O:10][CH3:11])=[C:8]([O:12][CH3:13])[CH:7]=7)=[CH:15][CH:16]=6)[CH2:25][CH2:24]5)[CH2:28][CH2:29]4)[CH2:35][CH2:36]3)=[O:59])=[CH:42][CH:43]=2)[CH:52]=[C:51]([O:53][CH3:54])[C:50]=1[O:55][CH3:56]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 15491076HCID 15491076, compound

Product 1

HCID 18770423HCID 18770423, compoundYield 83.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Concentrated hydrochloric acid (0.050 ml; 0.60 mmol) was added to a solution of the crude crystals of 1,4-bis[[4-[4-(3,4,5-trimethoxyphenyl)benzoyl]-1-piperazinyl]methyl]cyclohexane (118 mg; 0.14 mmol) in ethanol (5 ml) and the reaction mixture was concentrated under reduced pressure. After a process of adding ethanol (10 ml) to the residue and concentrating the mixture under reduced pressure was performed twice, the resultant concentrated residue was recrystallized from chloroform-methanol-diethyl ether to obtain 105 mg (yield: 58%) of the title compound as a pale yellow crystalline powder.

Workup

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. concentrationAfter a process of adding ethanol (10 ml) to the residue and concentrating the mixture under reduced pressure
  3. customthe resultant concentrated residue was recrystallized from chloroform-methanol-diethyl ether

Sources & evidence

ORD record
ord-9a4737a13e264134be1d1b96d4183bdf
Source dataset
uspto-grants-2002_09
Patent number
US06448242B1

Reaction notes

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