Sodium Hydroxide → HCID 68142496, compound

HRID 1076789Notes

Reaction equation

HRID 1076789 reaction equation
Cl.Cl.[C:3]1([CH:9]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][N:15]([CH2:18][C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[C:20]=3[O:29][CH3:30])[CH2:14][CH2:13]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[OH-].[Na+].O.[C:40]([OH:52])(=[O:51])[CH2:41][C:42]([CH2:47][C:48]([OH:50])=[O:49])([C:44]([OH:46])=[O:45])[OH:43]>O>[OH2:25].[C:40]([OH:52])(=[O:51])[CH2:41][C:42]([CH2:47][C:48]([OH:50])=[O:49])([C:44]([OH:46])=[O:45])[OH:43].[C:40]([OH:52])(=[O:51])[CH2:41][C:42]([CH2:47][C:48]([OH:50])=[O:49])([C:44]([OH:46])=[O:45])[OH:43].[C:31]1([CH:9]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:10][CH2:11][N:12]2[CH2:13][CH2:14][N:15]([CH2:18][C:19]3[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[C:21]([O:27][CH3:28])[C:20]=3[O:29][CH3:30])[CH2:16][CH2:17]2)[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 222302-Hydroxy-1,2,3-propanetricarboxylic acid hydrate (1:1)HCID 21537813HCID 21537813, compound

Product 1

HCID 68142496HCID 68142496, compoundYield 92.7%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

The amount of 6 g (0.011 mole) of 1-(3,3-diphenylpropyl)-4-(2,3,4-trimethoxybenzyl)piperazine dihydrochloride was dissolved in 50 ml of water, and 20 ml of a 10% sodium hydroxide solution was added. Then, the resulting solution was extracted three times, each time with 20 ml of ether, the ether layers combined, washed with water, and concentrated to a total volume of 10 ml. By adding a methanol-ether solution of 2.7 g (0.013 mole) of citric acid monohydrate to 5 ml of this concentrated solution, 4.4 g (92.7% yield) of 1-(3,3-diphenylpropyl)-4-(2,3,4-trimethoxybenzyl)piperazine dicitrate monohydrate with a melting point of 86° -92°C was obtained.

Workup

  1. extractionThen, the resulting solution was extracted three times
  2. washwashed with water
  3. concentrationconcentrated to a total volume of 10 ml

Sources & evidence

ORD record
ord-0884339e3f4d4865b9247de148fbd9d5
Source dataset
uspto-grants-1976_05
Patent number
US03957790

Reaction notes

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