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

HRID 1585464ノート

反応式

HRID 1585464 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-7719549e4b174447b74d31accaeae9a0
出典データセット
uspto-grants-1999_08
特許番号
US05939360

反応ノート

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