Hydrochloric Acid → HCID 18770409, compound

HRID 479412Notes

Reaction equation

HRID 479412 reaction equation
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([C:14]#[C:15]/[CH:16]=[CH:17]/[C:18]([N:20]2[CH2:25][CH2:24][N:23]([CH2:26][C:27]3[CH:32]=[CH:31][C:30]([CH2:33][N:34]4[CH2:39][CH2:38][N:37]([C:40](=[O:57])/[CH:41]=[CH:42]/[C:43]#[C:44][C:45]5[CH:50]=[C:49]([O:51][CH3:52])[C:48]([O:53][CH3:54])=[C:47]([O:55][CH3:56])[CH:46]=5)[CH2:36][CH2:35]4)=[CH:29][CH:28]=3)[CH2:22][CH2:21]2)=[O:19])[CH:7]=[C:8]([O:12][CH3:13])[C:9]=1[O:10][CH3:11]>C(O)C>[ClH:1].[ClH:1].[CH3:52][O:51][C:49]1[CH:50]=[C:45]([C:44]#[C:43]/[CH:42]=[CH:41]/[C:40]([N:37]2[CH2:38][CH2:39][N:34]([CH2:33][C:30]3[CH:31]=[CH:32][C:27]([CH2:26][N:23]4[CH2:22][CH2:21][N:20]([C:18](=[O:19])/[CH:17]=[CH:16]/[C:15]#[C:14][C:6]5[CH:7]=[C:8]([O:12][CH3:13])[C:9]([O:10][CH3:11])=[C:4]([O:3][CH3:2])[CH:5]=5)[CH2:25][CH2:24]4)=[CH:28][CH:29]=3)[CH2:35][CH2:36]2)=[O:57])[CH:46]=[C:47]([O:55][CH3:56])[C:48]=1[O:53][CH3:54]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 18770410HCID 18770410, compound

Product 1

HCID 18770409HCID 18770409, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Concentrated hydrochloric acid (0.055 ml; 0.66 mmol) was added to a solution of 1,4-bis[[4-[(E)-5-(3,4,5-trimethoxyphenyl)-2-penten-4-ynoyl]-1-piperazinyl]methyl]benzene (127 mg; 0.16 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 methylene chloride-methanol-diethyl ether to obtain 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 methylene chloride-methanol-diethyl ether

Sources & evidence

ORD record
ord-9458950e75674aa8bb9e793e10e99299
Source dataset
uspto-grants-2003_11
Patent number
US06645957B2

Reaction notes

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