Potassium Iodide → HCID 11043631、化合物

HRID 2393513ノート

反応式

HRID 2393513 の反応式
[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]

参加物

4

反応物 2

HCID 4875Potassium IodideHCID 18976125HCID 18976125、化合物

生成物 1

HCID 11043631HCID 11043631、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-a6f00ac1b3844fbdb885f65865435152
出典データセット
uspto-grants-1998_09
特許番号
US05807882

反応ノート

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