M-Cresol → 1-(Methoxymethoxy)-3-methylbenzene
반응식
[CH:1]1[C:6]([OH:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8].[H-].[Na+].[CH3:11][O:12][CH2:13]Cl>CN(C=O)C>[CH3:11][O:12][CH2:13][O:7][C:6]1[CH:5]=[CH:4][CH:3]=[C:2]([CH3:8])[CH:1]=1참가 물질
5
실험 절차
To m-cresol (19.4 mL, 188 mmol) in DMF (1 L) was added NaH (60% disp. in oil, 9.04 g, 0.226 mmol) in several portions. The mixture was stirred at rt for 30 min, chloromethyl methyl ether (11.5 mL, 151 mmol) was added in one portion, and the reaction mixture was stirred at room temperature overnight, partitioned between 1N aq. NaOH and Et2O. The organic phase was washed with 1N aq. NaOH, dried over MgSO4, filtered and concentrated in vacuo, to afford the title compound. 1H NMR (400 MHz, acetone-d6): 7.18 (t, 1H), 6.86-6.77 (m, 3H), 5.18 (s, 2H), 3.43 (s, 3H), 2.29 (s, 3H).
후처리
- stirringthe reaction mixture was stirred at room temperature overnight
- custompartitioned between 1N aq. NaOH and Et2O
- washThe organic phase was washed with 1N aq. NaOH
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-d7dc271f12e14c8ab2089bb87858de1e
- 출처 데이터셋
- uspto-grants-2011_06
- 특허 번호
- US07960409B2
반응 노트
불러오는 중…