1-Methylpiperazine → HCID 178480778, compound

HRID 437118Notes

Reaction equation

HRID 437118 reaction equation
Cl[C:2]1[NH:3][S:4](=[O:14])(=[O:13])[C:5]2[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:6]=2[N:7]=1.[CH3:15][N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>O>[Cl:12][C:10]1[CH:9]=[CH:8][C:6]2[N:7]=[C:2]([N:19]3[CH2:20][CH2:21][N:16]([CH3:15])[CH2:17][CH2:18]3)[NH:3][S:4](=[O:14])(=[O:13])[C:5]=2[CH:11]=1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 178527168HCID 178527168, compound

Product 1

HCID 178480778HCID 178480778, compoundYield 87.7%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

To a stirred suspension of 10.0 g of 3,7-dichloro-2H-1,2,4-benzothiadiazine 1,1-dioxide in 100 ml of water is added 8.0 g of 1-methylpiperazine, while the mixture is cooled in an ice bath. After the addition, the mixture is stirred at 60° C. for 1 hour. The crystalline precipitate collected is recrystallized from a mixture of dimethylformamide and water to give 11.0 g of the desired product, m.p. above 300° C.

Workup

  1. temperaturewhile the mixture is cooled in an ice bath
  2. additionAfter the addition
  3. customThe crystalline precipitate collected
  4. customis recrystallized from a mixture of dimethylformamide and water

Sources & evidence

ORD record
ord-f4730c105b7c40888b88cc38f25adc8e
Source dataset
uspto-grants-1977_06
Patent number
US04029780

Reaction notes

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