Diethyl Ether → P-Toluic Acid
반응식
Br([O-])(=O)=O.[Na+].[CH3:6][C:7]1[CH:14]=[CH:13][C:10]([CH2:11][OH:12])=[CH:9][CH:8]=1.CC[O:17]CC>C(#N)C.O>[CH3:6][C:7]1[CH:14]=[CH:13][C:10]([C:11]([OH:17])=[O:12])=[CH:9][CH:8]=1참가 물질
5
반응 조건
- 온도
- 80 °C
실험 절차
A mixture of Ceiv catalyst from Example 47 (0.08 g), sodium bromate (0.3 g) and 4-methylbenzyl alcohol (0.24 g, 2 mmol) in acetonitrile:water (1:1, 10 ml) was stirred at 80° C. for 40 h under an atmosphere of nitrogen. On cooling ether (70 ml) was added and the catalyst was filtered off. The organic layer was separated and the aqueous phase was extracted with ether (2×50 ml). The combined organic extracts were washed with water (25 ml), dried with anhydrous magnesium sulphate and concentrated to give 4-methylbenzoic acid as a white solid (0.26 g, 96%). M.p. 178° C., lit. 180-182° C.
후처리
- additionwas added
- filtrationthe catalyst was filtered off
- customThe organic layer was separated
- extractionthe aqueous phase was extracted with ether (2×50 ml)
- washThe combined organic extracts were washed with water (25 ml)
- dry with materialdried with anhydrous magnesium sulphate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-3a9fbafd96bf492091f8f6f9a3668ff1
- 출처 데이터셋
- uspto-grants-2010_06
- 특허 번호
- US07728159B2
반응 노트
불러오는 중…