Hydrochloric Acid → 3-Methyl-4-(trifluoromethyl)benzoic acid
반응식
[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]참가 물질
6
반응 조건
- 온도
- 23 °C
실험 절차
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].
후처리
- 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
출처 및 근거
- ORD 기록
- ord-2e27acf5057a456f9349af431d10cfd9
- 출처 데이터셋
- uspto-grants-2011_11
- 특허 번호
- US08063048B2
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