Potassium Iodide → HCID 20334282、化合物

HRID 1706715ノート

反応式

HRID 1706715 の反応式
[OH:1][C:2]1[C:11]([CH3:12])=[C:10]2[C:5]([C:6](=[O:15])[CH2:7][C:8]([CH3:14])([CH3:13])[O:9]2)=[CH:4][CH:3]=1.[CH2:16](Cl)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(=O)([O-])[O-:25].[K+].[K+].[I-].[K+]>CC(C)=O>[C:16]([O:1][C:2]1[C:11]([CH3:12])=[C:10]2[C:5]([C:6](=[O:15])[CH2:7][C:8]([CH3:13])([CH3:14])[O:9]2)=[CH:4][CH:3]=1)(=[O:25])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 27279747-Hydroxy-2,2,8-trimethyl-2,3-dihydro-4H-1-benzopyran-4-one

生成物 1

HCID 20334282HCID 20334282、化合物収率 82.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

The mixture of 10.3 g. of the compound obtained in (1), 8.2 g. of benzyl chloride, 10.2 g. of potassium carbonate, 0.5 g. of potassium iodide, and 100 ml of acetone was refluxed for 2 hours. The mixture was then filtered, and the filtrate was concentrated. Ether was added to the concentrate. The ether layer was washed successively with water, 1 N aqueous sodium hydroxide, and again with water. The solution was dried over magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane, to obtain 12.2 g. (yield: 82.4%) of the subject compound.

後処理

  1. additionThe mixture of 10.3 g
  2. filtrationThe mixture was then filtered
  3. concentrationthe filtrate was concentrated
  4. additionEther was added to the concentrate
  5. washThe ether layer was washed successively with water, 1 N aqueous sodium hydroxide
  6. dry with materialThe solution was dried over magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure
  8. customThe residue was recrystallized from ethyl acetate/n-hexane
  9. customto obtain 12.2 g

出典と根拠

ORDレコード
ord-d6c4c24cf436424cb038d0ab6a3520ad
出典データセット
uspto-grants-1980_06
特許番号
US04208426

反応ノート

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