참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl morpholine oxide | HCID 82029 | — |
| 반응물 | Methyl 3,5-dibromo-4-(bromomethyl)benzoate | HCID 22647948 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | Methyl 3,5-dibromo-4-formylbenzoate | HCID 22647908 | — |
반응 단계
Methyl 3,5-dibromo-4-(bromomethyl)benzoate (INTERMEDIATE 24) (3.9 g) was dissolved in acetonitrile (100 mL) and to this was added 4 Å molecular sieves and N-methylmorpholine N-oxide (1.18 g) and the reaction heated to 50° C. for 12 h. The reaction mixture was poured into brine and extracted into ethyl acetate, dried over MgSO4 and concentrated. The residue was purified by silica gel chromatography eluting with 90% hexane:10% ethyl acetate to give the title compound. 1H NMR (500 MHz, CDCl3): δ 10.27 (s, 1H); 8.29 (s, 2H); 3.99 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06809199B2 |
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| 출처 데이터셋 | uspto-grants-2004_10 |
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| ORD ID | ord-552b45866d3a478b82a8275088fb5393 |
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| 출처 메모 | uspto-grants-2004_10 |
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