Trifluoroacetic acid → Methyl 3-hydroxy-5-(4-(methylsulfonyl)phenoxy)benzoate

HRID 2113823ノート

反応式

HRID 2113823 の反応式
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10](=[O:32])[C:11]1[CH:16]=[C:15]([O:17]COC)[CH:14]=[C:13]([O:21][C:22]2[CH:27]=[CH:26][C:25]([S:28]([CH3:31])(=[O:30])=[O:29])=[CH:24][CH:23]=2)[CH:12]=1>C(Cl)Cl>[CH3:8][O:9][C:10](=[O:32])[C:11]1[CH:16]=[C:15]([OH:17])[CH:14]=[C:13]([O:21][C:22]2[CH:23]=[CH:24][C:25]([S:28]([CH3:31])(=[O:29])=[O:30])=[CH:26][CH:27]=2)[CH:12]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 592633143-(4-Methanesulfonyl-phenoxy)-5-methoxymethoxy-benzoic acid methyl ester

生成物 1

HCID 46941846Methyl 3-hydroxy-5-(4-(methylsulfonyl)phenoxy)benzoate収率 56%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

After adding 60 ml of trifluoroacetic acid to a solution of 30.9 g (84.3 mmol) of the obtained 3-(4-methanesulfonyl-phenoxy)-5-methoxymethoxy-benzoic acid methyl ester in methylene chloride (100 ml) while cooling on ice, the reaction mixture was stirred at room temperature for 4 hours. The reaction mixture was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (hexane:acetic acid ethyl ester=1:1) to obtain 15.2 g of 5-hydroxy-3-(4-methanesulfonyl-phenoxy)benzoic acid methyl ester (yield: 56%) as a white solid.

後処理

  1. temperaturewhile cooling on ice
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customthe obtained residue was purified by silica gel column chromatography (hexane:acetic acid ethyl ester=1:1)

出典と根拠

ORDレコード
ord-1f6b4700085c4bc0a33456e44ff292b5
出典データセット
uspto-grants-2008_10
特許番号
US07432287B2

反応ノート

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