反応式
C[O:2][C:3](=[O:20])[CH2:4][S:5](=[O:19])(=[O:18])[NH:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[C:14]([F:17])([F:16])[F:15].[OH-].[Na+].Cl>O1CCOCC1>[F:13][C:10]1[CH:11]=[CH:12][C:7]([NH:6][S:5]([CH2:4][C:3]([OH:20])=[O:2])(=[O:19])=[O:18])=[C:8]([C:14]([F:17])([F:15])[F:16])[CH:9]=1参加物
5
実験手順
2.2 g (6.98 mmol) of 2-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]acetic acid methyl ester is dissolved in 20 ml of dioxane, and the solution is combined with 10 ml (20 mmol) of 2N sodium hydroxide solution. The mixture heats up slightly, and saponification is completed after 10 minutes. The solution is neutralized with 2N hydrochloric acid under pH control and gently evaporated to dryness under vacuum. The residue is extracted with 30 ml of ethyl acetate, the solution is extracted once by shaking with 10 ml of water, the organic phase is dried over magnesium sulfate, filtered, and evaporated to dryness, thus obtaining 1.96 g (6.51 mmol)=93.2% of theory.
後処理
- customgently evaporated to dryness under vacuum
- extractionThe residue is extracted with 30 ml of ethyl acetate
- extractionthe solution is extracted once
- dry with materialthe organic phase is dried over magnesium sulfate
- filtrationfiltered
- customevaporated to dryness
- customthus obtaining 1.96 g (6.51 mmol)=93.2% of theory
出典と根拠
- ORDレコード
- ord-cbda5d5848914e98969cbceb8642d5f2
- 出典データセット
- uspto-grants-1993_05
- 特許番号
- US05210290
関連ノート
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