Pyridine → Methyl 4-methanesulfonyl-2-methyl-3-(trifluoromethanesulfonyl)oxybenzoate

HRID 1585464노트

반응식

HRID 1585464 반응식
[OH:1][C:2]1[C:3]([CH3:16])=[C:4]([CH:9]=[CH:10][C:11]=1[S:12]([CH3:15])(=[O:14])=[O:13])[C:5]([O:7][CH3:8])=[O:6].N1C=CC=CC=1.[F:23][C:24]([F:30])([F:29])[S:25](O)(=[O:27])=[O:26]>C(Cl)Cl>[CH3:15][S:12]([C:11]1[CH:10]=[CH:9][C:4]([C:5]([O:7][CH3:8])=[O:6])=[C:3]([CH3:16])[C:2]=1[O:1][S:25]([C:24]([F:30])([F:29])[F:23])(=[O:27])=[O:26])(=[O:14])=[O:13]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 62406Trifluoromethanesulfonic acidHCID 18694846Methyl 3-hydroxy-4-methanesulfonyl-2-methylbenzoate

생성물 1

HCID 18694857Methyl 4-methanesulfonyl-2-methyl-3-(trifluoromethanesulfonyl)oxybenzoate수율 99.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

8.8 g (0.036 mol) of methyl 3-hydroxy-4-methanesulfonyl-2-methyl-benzoate was dissolved in 100 ml of methylene chloride, and 8.3 g (0.11 mol) of pyridine was added. After the solution was cooled to 0° C., 12.2 g (0.043 mol) of anhydrous trifluoromethanesulfonic acid was added. After stirring at room temperature for 1 hour, the reaction mixture was washed with 1N hydrochloric acid and subsequently with saturated sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 13.5 g of methyl 4-methanesulfonyl-2-methyl-3-(trifluoromethanesulfonyl)oxybenzoate. Yield=99%.

후처리

  1. washthe reaction mixture was washed with 1N hydrochloric acid and subsequently with saturated sodium chloride solution
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-7719549e4b174447b74d31accaeae9a0
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05939360

반응 노트

불러오는 중…