Methanesulfonic Acid → HCID 18770443, compound

HRID 479407Notes

Reaction equation

HRID 479407 reaction equation
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:9]=[C:10]([C:18]2[CH:61]=[CH:60][C:21]([C:22]([N:24]3[CH2:29][CH2:28][N:27]([CH2:30][CH2:31][CH2:32][CH2:33][N:34]4[CH2:39][CH2:38][N:37]([C:40](=[O:59])[C:41]5[CH:46]=[CH:45][C:44]([C:47]6[CH:52]=[C:51]([O:53][CH3:54])[C:50]([O:55][CH3:56])=[C:49]([O:57][CH3:58])[CH:48]=6)=[CH:43][CH:42]=5)[CH2:36][CH2:35]4)[CH2:26][CH2:25]3)=[O:23])=[CH:20][CH:19]=2)[CH:11]=[C:12]([O:16][CH3:17])[C:13]=1[O:14][CH3:15]>C(O)C>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[CH3:54][O:53][C:51]1[CH:52]=[C:47]([C:44]2[CH:43]=[CH:42][C:41]([C:40]([N:37]3[CH2:38][CH2:39][N:34]([CH2:33][CH2:32][CH2:31][CH2:30][N:27]4[CH2:28][CH2:29][N:24]([C:22](=[O:23])[C:21]5[CH:60]=[CH:61][C:18]([C:10]6[CH:9]=[C:8]([O:7][CH3:6])[C:13]([O:14][CH3:15])=[C:12]([O:16][CH3:17])[CH:11]=6)=[CH:19][CH:20]=5)[CH2:25][CH2:26]4)[CH2:35][CH2:36]3)=[O:59])=[CH:46][CH:45]=2)[CH:48]=[C:49]([O:57][CH3:58])[C:50]=1[O:55][CH3:56]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 15491074HCID 15491074, compound

Product 1

HCID 18770443HCID 18770443, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A 0.1 M aqueous solution of methanesulfonic acid (3.0 ml; 0.30 mmol) was added to a solution of 1,4-bis[4-[4-(3,4,5-trimethoxyphenyl)benzoyl]-1-piperazinyl]butane (110 mg; 0.14 mmol) in ethanol (15 ml) and the reaction mixture was concentrated under reduced pressure. After a process of adding ethanol (15 ml) to the residue and concentrating the mixture under reduced pressure was performed 3 times, the resultant concentrated residue was recrystallized from methanol-diethyl ether to obtain the title compound as colorless prisms.

Workup

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. concentrationAfter a process of adding ethanol (15 ml) to the residue and concentrating the mixture under reduced pressure
  3. customthe resultant concentrated residue was recrystallized from methanol-diethyl ether

Sources & evidence

ORD record
ord-710a6fe793bb496bbe70d2b9b9a2c2a0
Source dataset
uspto-grants-2003_11
Patent number
US06645957B2

Reaction notes

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