Potassium Carbonate → 1-Methanesulfonyl-3,3-dimethylpiperazine

HRID 465924Notes

Reaction equation

HRID 465924 reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][C:7]1([CH3:13])[CH2:12][NH:11][CH2:10][CH2:9][NH:8]1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH3:1][S:2]([N:11]1[CH2:10][CH2:9][NH:8][C:7]([CH3:13])([CH3:6])[CH2:12]1)(=[O:4])=[O:3]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 146641862,2-Dimethylpiperazine

Product 1

HCID 198151421-Methanesulfonyl-3,3-dimethylpiperazine

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

A solution of 52.8 g of methanesulphonyl chloride in 100 ml of toluene is added dropwise to a mixture of 52.6 g of 2,2-dimethylpiperazine, 69.9 g of potassium carbonate and 150 ml of toluene, the internal temperature rising to about 55° C. After a stirring time of 3 hours, the insoluble fraction is filtered off with suction and the toluene solution is evaporated in vacuo. The oil which remains gradually solidifies and is recrystallised from isopropanol for purification.

Workup

  1. customrising to about 55° C
  2. filtrationAfter a stirring time of 3 hours, the insoluble fraction is filtered off with suction
  3. customthe toluene solution is evaporated in vacuo
  4. customis recrystallised from isopropanol for purification

Sources & evidence

ORD record
ord-13fb563f71bb4756a333355efe592e55
Source dataset
uspto-grants-1992_10
Patent number
US05155109

Reaction notes

Loading…