참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | (4-Bromo-3,5-dimethoxyphenyl)methanol | HCID 11149289 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 2-Bromo-1,3-dimethoxy-5-(methoxymethyl)benzene | HCID 23080940 | — |
반응 단계
Sodium hydride (60% in oil; 24.7 g) was added to a solution of (4-bromo-3,5-dimethoxyphenyl)methanol (118.8 g) in N,N-dimethylformamide (960 mL) while cooling with ice, and after stirring for 10 minutes, iodomethane (41.7 mL) was added dropwise, the temperature was increased to room temperature and stirring was continued for 1 hour. The obtained reaction mixture was poured into ice water (2.5 L), extraction was performed with ethyl acetate, the extract was washed with brine and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography and the title compound (121.3 g) was obtained as a colorless oil from the n-hexane:ethyl acetate (4:1) fraction.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07176216B2 |
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| 출처 데이터셋 | uspto-grants-2007_02 |
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| ORD ID | ord-8de60d3a532e4ce8a40c12f13e2c0ca7 |
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| 출처 메모 | uspto-grants-2007_02 |
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