Hydrochloric Acid → HCID 15030536, compound

HRID 1589979Notes

Reaction equation

HRID 1589979 reaction equation
[C:1]([CH:4]1[C:8](=[O:9])[CH:7]([CH3:10])[CH2:6][S:5]1)(=[O:3])[CH3:2].S(Cl)(Cl)(=O)=O.S(Cl)(Cl)(=O)=O.C(Cl)Cl.Cl>C(Cl)Cl.O>[C:1]([C:4]1[S:5][CH:6]=[C:7]([CH3:10])[C:8]=1[OH:9])(=[O:3])[CH3:2]

Participants

7

Reactant 4

HCID 313Hydrochloric AcidHCID 24648Sulfuryl chlorideHCID 15030535HCID 15030535, compoundHCID 86746693HCID 86746693, compound

Product 1

HCID 15030536HCID 15030536, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent2×

Procedure

36.0 g (0.227 mol) of 2-acetyl-3-keto-4-methyl-4,5-dihydrothiophene are initially introduced into 260 ml of methylene chloride 21.9 ml of sulphuryl chloride in 260 ml of methylene chloride are then added dropwise at 0° C. While the sulphuryl chloride/methylene chloride mixture is added dropwise, a stream of nitrogen is passed into the solution to expel the HCl gas which is formed. When the addition is complete, stirring is continued for 30 minutes at 10°-15° C. The mixture is then introduced into 600 ml of water, and the organic phase is extracted with a 5% strength NaHCO3 solution, dried and concentrated in vacuo.

Workup

  1. additionare then added dropwise at 0° C
  2. customis formed
  3. additionWhen the addition
  4. extractionthe organic phase is extracted with a 5% strength NaHCO3 solution
  5. customdried
  6. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-408d6fe5ad8a4bc5ac3cf18a4e9f09ea
Source dataset
uspto-grants-1993_04
Patent number
US05201936

Reaction notes

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