Triethylamine → HCID 13120686, compound

HRID 745235Notes

Reaction equation

HRID 745235 reaction equation
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]1[NH:11][CH2:10][CH2:9][NH:8][C:7]1=[O:12].C(N(CC)CC)C.[CH3:20][N:21]([CH3:26])[S:22](Cl)(=[O:24])=[O:23]>C(Cl)(Cl)Cl>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]1[N:11]([S:22]([N:21]([CH3:26])[CH3:20])(=[O:24])=[O:23])[CH2:10][CH2:9][NH:8][C:7]1=[O:12]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 65649Piperazinone, 3-(2-thienyl)- (9CI)HCID 83372Dimethylsulphamoyl chloride

Product 1

HCID 13120686HCID 13120686, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

9.1 g (0.05 mol) of 3-(2-thienyl)-piperazin-2-one, prepared in accordance with Example 16, are mixed with a solution of 6.1 g (0.06 mol) of triethylamine in 100 ml of chloroform, and 8.6 g (0.06 mol) of dimethylaminosulphonyl chloride are added dropwise slowly. The reaction mixture is then stirred for a further 6 hours at room temperature and evaporated in vacuo, the residue is stirred with water and the mixture is extracted by shaking with ethyl acetate. The ethyl acetate phase is separated off, the ethyl acetate is removed by distillation and the residue is recrystallised from ethanol.

Workup

  1. additionare added dropwise slowly
  2. customevaporated in vacuo
  3. stirringthe residue is stirred with water
  4. extractionthe mixture is extracted
  5. stirringby shaking with ethyl acetate
  6. customThe ethyl acetate phase is separated off
  7. customthe ethyl acetate is removed by distillation
  8. customthe residue is recrystallised from ethanol

Sources & evidence

ORD record
ord-af0a42b51ffb4df584687e11d6ea6409
Source dataset
uspto-grants-1986_07
Patent number
US04598079

Reaction notes

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