Potassium Iodide → HCID 20334282, 화합물

HRID 1706715노트

반응식

HRID 1706715 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 20334282HCID 20334282, 화합물수율 82.4%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d6c4c24cf436424cb038d0ab6a3520ad
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04208426

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