HCID 20096447, compound → HCID 20096464, compound

HRID 1769969Notes

Reaction equation

HRID 1769969 reaction equation
[C:1]([O-:4])(=[S:3])[CH3:2].[K+].Cl[CH2:7][C:8]1[C:16]2[S:15][N:14]=[N:13][C:12]=2[CH:11]=[CH:10][CH:9]=1>CS(C)=O>[C:1]([S:3][CH2:7][C:8]1[C:16]2[S:15][N:14]=[N:13][C:12]=2[CH:11]=[CH:10][CH:9]=1)(=[O:4])[CH3:2]

Participants

4

Reactant 2

HCID 20096447HCID 20096447, compoundHCID 23670855Potassium ethanethioate

Product 1

HCID 20096464HCID 20096464, compound

Reagents, catalysts & solvents 1

HCID 679Dimethyl SulfoxideSolvent2×

Procedure

A solution of 2.2 g of potassium thioacetate in 20 ml of absolute dimethyl sulfoxide, stirred at 20° C., is treated dropwise with stirring with a solution of 2.8 g of 7-chloromethylbenzo-1,2,3-thiadiazole in 10 ml of dimethyl sulfoxide, during which process the internal temperature rises to 37° C. The mixture is subsequently stirred overnight at room temperature and, on the following day, poured into ice-water and extracted using ethyl acetate. The extracts are washed five times with water, dried over sodium sulfate and evaporated. The residue which remains is distilled in vacuo, resulting in an oil of refractive index nd27 -1.6478.

Workup

  1. additionis treated dropwise
  2. customrises to 37° C
  3. extractionextracted
  4. washThe extracts are washed five times with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. distillationThe residue which remains is distilled in vacuo
  8. customresulting in an oil of refractive index nd27 -1.6478

Sources & evidence

ORD record
ord-9b53871f95814cba8fbc0e1f125e8d4a
Source dataset
uspto-grants-1995_01
Patent number
US05384321

Reaction notes

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