Potassium Carbonate → 1-(5'-Ethoxymethoxy-2'methyl-2-propylbiphenyl-4-yl)propan-1-one

HRID 584287노트

반응식

HRID 584287 반응식
[CH2:1]([O:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:15])=[C:10](B(O)O)[CH:11]=1)[CH3:2].FC(F)(F)S(O[C:22]1[CH:27]=[CH:26][C:25]([C:28](=[O:31])[CH2:29][CH3:30])=[CH:24][C:23]=1[CH2:32][CH2:33][CH3:34])(=O)=O.[Cl-].[Li+].C(=O)([O-])[O-].[K+].[K+]>COCCOC.O>[CH2:1]([O:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:15])=[C:10]([C:22]2[CH:27]=[CH:26][C:25]([C:28](=[O:31])[CH2:29][CH3:30])=[CH:24][C:23]=2[CH2:32][CH2:33][CH3:34])[CH:11]=1)[CH3:2]

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 433294Lithium ChlorideHCID 223456045-Ethoxymethoxy-2-methylphenylboronic acidHCID 223456254-Propionyl-2-propylphenyl 1,1,1-trifluoromethanesulfonate

생성물 1

HCID 223456341-(5'-Ethoxymethoxy-2'methyl-2-propylbiphenyl-4-yl)propan-1-one

시약·촉매·용매 2

HCID 962Water용매HCID 80711,2-Dimethoxyethane용매

실험 절차

1.56 g (7.4 mmol) of 5-ethoxymethoxy-2-methylphenylboronic acid, 2 g (6.2 mmol) of 4-propionyl-2-propylphenyl 1,1,1-trifluoromethanesulfonate, 517 mg (12 mmol) of lithium chloride and 7.4 ml of 2M potassium carbonate solution are dissolved in 50 ml of 1,2-dimethoxyethane in a round-bottomed flask and under a stream of nitrogen. The mixture is refluxed for 10 hours. It is then poured into water and extracted with ethyl acetate. The organic phase is dried over magnesium sulfate, filtered and then evaporated. A brown oil is obtained, which is used without further purification for the rest of the synthesis.

후처리

  1. temperatureThe mixture is refluxed for 10 hours
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customA brown oil is obtained
  7. customwhich is used without further purification for the rest of the synthesis

출처 및 근거

ORD 기록
ord-38af767a9938472f8beb49ae44c4f95f
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06924400B2

반응 노트

불러오는 중…