Chloromethyl Methyl Ether → 1-Bromo-3-[(methoxymethoxy)methyl]benzene
반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH2:5][OH:6].[H-].[Na+].[CH3:12][O:13][CH2:14]Cl>O1CCCC1>[Br:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:4]([CH2:5][O:6][CH2:12][O:13][CH3:14])[CH:3]=1참가 물질
5
반응 조건
- 온도
- 60 °C
실험 절차
To a tetrahydrofuran (100 mL) solution of 3-bromobenzyl alcohol (10 g, 54 mmol) was added sodium hydride (2.3 g, 98 mmol, 60% in oil) at room temperature. Then, chloromethyl methyl ether (5.2 g, 64 mmol) was added to this suspension, which was stirred for 15 minutes at 60° C. This mixture was partitioned into ethyl acetate and water. The organic layer was separated and concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=8:1) to obtain the title compound (10 g, 83%).
후처리
- customThis mixture was partitioned into ethyl acetate and water
- customThe organic layer was separated
- concentrationconcentrated under a reduced pressure
- customThe residue was purified by silica gel column chromatography (heptane:ethyl acetate=8:1)
출처 및 근거
- ORD 기록
- ord-4203a6b99c9c41c7b61a2107c2ecb1da
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08841327B2
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