Potassium Iodide → HCID 11043631, compound

HRID 2393513Notes

Reaction equation

HRID 2393513 reaction equation
[C:1]([O:4][C:5]1[CH:21]=[CH:20][C:8]2[O:9][C:10](Br)([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH:11](Br)[O:12][C:7]=2[CH:6]=1)(=[O:3])[CH3:2].[I-].[K+]>CC(C)=O>[C:1]([O:4][C:5]1[CH:21]=[CH:20][C:8]2[O:9][C:10]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:11][O:12][C:7]=2[CH:6]=1)(=[O:3])[CH3:2]

Participants

4

Procedure

Under an inert atmosphere, 6 g of ethyl 6-acetoxy-2,3-dibromo- 1,4-benzodioxane-2-carboxylate in solution in 100 ml of acetone are mixed with 7.75 g of potassium iodide and stirred for 6 hours. After evaporation of the acetone under reduced pressure, the residue is diluted in ether and then washed with 20% sodium thiosulfate solution until the mixture is decolorized. The organic phase is then dried over magnesium sulfate and thereafter concentrated under vacuum. The compound is purified by chromatography on silica gel (eluent: petroleum ether/ethyl acetate, 7:3).

Workup

  1. customAfter evaporation of the acetone under reduced pressure
  2. additionthe residue is diluted in ether
  3. washwashed with 20% sodium thiosulfate solution until the mixture
  4. dry with materialThe organic phase is then dried over magnesium sulfate
  5. concentrationconcentrated under vacuum
  6. customThe compound is purified by chromatography on silica gel (eluent: petroleum ether/ethyl acetate, 7:3)

Sources & evidence

ORD record
ord-a6f00ac1b3844fbdb885f65865435152
Source dataset
uspto-grants-1998_09
Patent number
US05807882

Reaction notes

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