Isopropyl iodide → 5-Hydroxy-7-isopropoxy-2-methylthiochromone

HRID 2209661노트

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HRID 2209661 반응식
[OH:1][C:2]1[CH:11]=[C:10]([OH:12])[CH:9]=[C:8]2[C:3]=1[C:4](=[S:14])[CH:5]=[C:6]([CH3:13])[O:7]2.C(=O)([O-])[O-].[K+].[K+].[CH:21](I)([CH3:23])[CH3:22]>CN(C=O)C>[OH:1][C:2]1[CH:11]=[C:10]([O:12][CH:21]([CH3:23])[CH3:22])[CH:9]=[C:8]2[C:3]=1[C:4](=[S:14])[CH:5]=[C:6]([CH3:13])[O:7]2

참가 물질

5

반응물 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 1361024115,7-Dihydroxy-2-methylthiochromone

생성물 1

HCID 1361364155-Hydroxy-7-isopropoxy-2-methylthiochromone수율 88.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

A mixture consisting of 6.88 g (30.35 mmol) 5,7-dihydroxy-2-methylthiochromone, 12.56 g (91.05 mmol) potassium carbonate, 6.07 ml (60.70 mmol) isopropyl iodide, and 150 ml DMF was stirred at 60° C. for 30 min. Subsequently, 5 added to the solution thus reacted. The product was extracted twice with ethyl acetate. organic layer was washed with saturated salt water and dried over sodium sulfate anhydride. The solvent was distilled out under reduced pressure. The resulting crude product was purified by flash column cliromatography (hexane ethyl acetate =4:1), whereby 6.71 g of 5-hydroxy-7-isopropoxy-2-methylthiochromone was obtained (yield: 83%).

후처리

  1. additionSubsequently, 5 added to the solution
  2. customthus reacted
  3. extractionThe product was extracted twice with ethyl acetate
  4. washorganic layer was washed with saturated salt water
  5. dry with materialdried over sodium sulfate anhydride
  6. distillationThe solvent was distilled out under reduced pressure
  7. customThe resulting crude product was purified by flash column cliromatography (hexane ethyl acetate =4:1)

출처 및 근거

ORD 기록
ord-02ee9af36fd8431e8b20c02648ac837f
출처 데이터셋
uspto-grants-1995_10
특허 번호
US05455267

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