참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Bromomethyl methyl ether | HCID 83093 | — |
| 반응물 | 1-Bromo-4-chloro-2-fluorobenzene | HCID 137275 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-Bromo-4-chloro-2-fluoro-3-(methoxymethyl)benzene | HCID 68809381 | 71% |
반응 단계
A solution of 1-bromo-4-chloro-2-fluorobenzene (20.4 g, 0.100 mol) in THF (50 mL) was slowly added to LDA (0.125 mol) in THF (600 mL) at −50° C. After addition the solution was warmed to −20° C. and then cooled to −50° C. a solution of bromomethoxymethane (25 g, 0.200 mol) in THF (25 mL) was slowly added and the reaction mixture was warmed to ambient temperature. The reaction was quenched with water (400 mL) and extracted with diethyl ether (2×150 mL). The combined organic phases were dried (sodium sulfate) and concentrated. The residual oil was distilled (70°-75° C./0.5 mm) to give 1-bromo-4-chloro-2-fluoro-3-methoxymethylbenzene (18.0 g, 0.071 mol): 1H NMR (CDCl3): δ 7.50 (m, 1H), 7.15 (dd, 1H), 4.65 (s, 1H), 3.40 (s, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07498468B2 |
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| 출처 데이터셋 | uspto-grants-2009_03 |
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| ORD ID | ord-3a11670a4488410a9c3499f7a22e5f03 |
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| 출처 메모 | uspto-grants-2009_03 |
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