참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 2,2-Dimethoxypropane | HCID 6495 | — |
| 반응물 | 4-(4-Bromophenyl)-2,2-dimethyl-4-oxo-butyric Acid | HCID 21985757 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Methyl 4-(4-bromophenyl)-2,2-dimethyl-4-oxobutanoate | HCID 21985797 | — |
반응 단계
To a solution of 4-(4-bromophenyl)-2,2-dimethyl-4-oxobutanoic acid (8.33 g, 29.2 mmol) and 2,2-dimethoxypropane (3.95 g, 37.9 mmol) in methanol (100 mL) was added 1 M HCl in dioxane (2.0 mL). The reaction mixture was stirred at 50° C. for 22 h. The mixture was concentrated under reduced pressure. Toluene (2×60 mL) was added and the mixture concentrated again (2×) to afford methyl 4-(4-bromophenyl)-2,2-dimethyl-4-oxobutanoate as an off-white, semi-solid (8.60 g, 99%). This material was used in the next step without further purification. LC-MS: ret. time 3.23 min; m/z 298.8 (MH+); 1H NMR (300 MHz, CDCl3) δ 1.34 (s, 6H), 3.28 (s, 2H), 3.67 (s, 3H), 7.58 (d, 2H), 7.78 (d, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07423156B2 |
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| 출처 데이터셋 | uspto-grants-2008_09 |
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| ORD ID | ord-c98b80f9941846d5970ca84f6b0e2968 |
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| 출처 메모 | uspto-grants-2008_09 |
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