Ethyl Acetate → HCID 18930898, compound

HRID 1599209Notes

Reaction equation

HRID 1599209 reaction equation
Cl[S:2]([C:5]1[S:6][C:7]([Cl:13])=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)(=[O:4])=[O:3].[F-:14].[K+].C(OCC)(=O)C>O1CCOCC1.O>[F:14][S:2]([C:5]1[S:6][C:7]([Cl:13])=[C:8]([N+:10]([O-:12])=[O:11])[CH:9]=1)(=[O:4])=[O:3]

Participants

6

Reactant 3

HCID 8857Ethyl AcetateHCID 522689Potassium FluorideHCID 27357835-Chloro-4-nitrothiophene-2-sulfonyl chloride

Product 1

HCID 18930898HCID 18930898, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 312751,4-DioxaneSolvent

Conditions

Temperature
50 °C

Procedure

2--Chlorosulphonyl-4-nitro-5-chlorothiophene (20.1 parts) were stirred in p-dioxane (80 parts) at room temperature. Potassium fluoride (5.2 parts) in water (20 parts) was added and the mixture heated to 50° C. Stirred under these conditions for 4 hours, then cooled and poured onto ice/water. Ethyl acetate was then added to extract the product and separated. Dried over magnessium sulphate then screened and concentrated to yield the product 2-fluorosulphonyl-4-nitro-5-chloro thiophene (20.4 parts).

Workup

  1. temperaturecooled
  2. additionpoured onto ice/water
  3. extractionto extract the product
  4. customseparated
  5. dry with materialDried over magnessium sulphate
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-828e6de827884b62b3e7c1dba8aa0155
Source dataset
uspto-grants-1998_04
Patent number
US05739299

Reaction notes

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