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Sodium Hydroxide → Rac-5-methylsulfamoyl-2-(2,2,2-trifluoro-1-methyl-ethoxy)-benzoic acid

HRID 1820790
ノート
印刷プレビュー

反応式

HRID 1820790 の反応式
C[O:2][C:3](=[O:22])[C:4]1[CH:9]=[C:8]([S:10](=[O:14])(=[O:13])[NH:11][CH3:12])[CH:7]=[CH:6][C:5]=1[O:15][CH:16]([CH3:21])[C:17]([F:20])([F:19])[F:18].[OH-].[Na+]>C1COCC1>[CH3:12][NH:11][S:10]([C:8]1[CH:7]=[CH:6][C:5]([O:15][CH:16]([CH3:21])[C:17]([F:19])([F:18])[F:20])=[C:4]([CH:9]=1)[C:3]([OH:22])=[O:2])(=[O:13])=[O:14]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 577534755-Methylsulfamoyl-2-(2,2,2-trifluoro-1-methyl-ethoxy)-benzoic acid methyl ester

生成物 1

HCID 57753718Rac-5-methylsulfamoyl-2-(2,2,2-trifluoro-1-methyl-ethoxy)-benzoic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

To 1.6 mmol 5-methylsulfamoyl-2-(2,2,2-trifluoro-1-methyl-ethoxy)-benzoic acid methyl ester in 10 ml THF was added 20 mmol 2 M aq NaOH, and the mixture was heated at 50° C. for 2 h. The mixture was then cooled to RT and extracted twice with ether. The aqueous phase was acidified with 10% aq citric acid and extracted twice with ethyl acetate. The combined organic phases were dried with Na2SO4. Evaporation in vacuo followed by trituration in ether and hexane afforded the title compound. MS (m/e): 326.2 ([M−H]−, 100%)

後処理

  1. temperatureThe mixture was then cooled to RT
  2. extractionextracted twice with ether
  3. extractionextracted twice with ethyl acetate
  4. dry with materialThe combined organic phases were dried with Na2SO4
  5. customEvaporation in vacuo

出典と根拠

ORDレコード
ord-fd4e82e3e17640b08c2490430e35fcc0
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07605163B2

反応ノート

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