Hydrochloric Acid → 3-Methyl-4-(trifluoromethyl)benzoic acid
反応式
[CH3:1][C:2]1[CH:3]=C([CH:7]=[CH:8][C:9]=1[C:10]([F:13])([F:12])[F:11])C#N.[OH-:14].[Na+].Cl.[O:17]1[CH2:22][CH2:21]OCC1>CC(OC)(C)C>[CH3:1][C:2]1[CH:3]=[C:21]([CH:7]=[CH:8][C:9]=1[C:10]([F:13])([F:12])[F:11])[C:22]([OH:17])=[O:14]参加物
6
反応条件
- 温度
- 23 °C
実験手順
A mixture of 3-methyl-4-trifluoromethyl-benzonitrile from step 5 (16.25 g, 88 mmol) and 3 N NaOH (88 mL, 264 mmol) in dioxane (90 mL) was refluxed for 18 h. The mixture was cooled to 23° C., diluted with TBME, acidified with 1 N HCl to pH 1 and extracted twice with TBME. The combined organic layers were washed with brine, dried over MgSO4. Removal of the solvent in vacuum left the title compound as an off white solid (14.46 g, 81%), which was used without further purification. MS (ISN) 203.1 [M−H].
後処理
- temperaturewas refluxed for 18 h
- extractionextracted twice with TBME
- washThe combined organic layers were washed with brine
- dry with materialdried over MgSO4
- customRemoval of the solvent in vacuum
- waitleft the title compound as an off white solid (14.46 g, 81%), which
- customwas used without further purification
出典と根拠
- ORDレコード
- ord-2e27acf5057a456f9349af431d10cfd9
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063048B2
反応ノート
読み込み中…