1-Methylpiperazine → HCID 178480777, compound

HRID 437119Notes

Reaction equation

HRID 437119 reaction equation
Cl[C:2]1[NH:3][S:4](=[O:13])(=[O:12])[C:5]2[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=2[N:7]=1.[CH3:14][N:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1>CO>[CH3:14][N:15]1[CH2:20][CH2:19][N:18]([C:2]2[NH:3][S:4](=[O:13])(=[O:12])[C:5]3[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=3[N:7]=2)[CH2:17][CH2:16]1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 178527167HCID 178527167, compound

Product 1

HCID 178480777HCID 178480777, compoundYield 72.2%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a stirred suspension of 10.7 g of 3-chloro-2H-1,2,4-benzothiadiazine 1,1-dioxide in 100 ml of methanol is added 9.9 g of 1-methylpiperazine and the mixture is heated under reflux for 2 hours. After cooling, the crystalline precipitate is collected by suction filtration and recrystallized from a mixture of dimethylformamide and water to give 10.0 g of the desired product, m.p. 265°-267° C.

Workup

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling
  4. filtrationthe crystalline precipitate is collected by suction filtration
  5. customrecrystallized from a mixture of dimethylformamide and water

Sources & evidence

ORD record
ord-f4ffade032284a0bbe823ab241b20e15
Source dataset
uspto-grants-1977_06
Patent number
US04029780

Reaction notes

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