참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Propanoic acid, 2-bromo-2-methyl-, ethyl ester | HCID 11745 | — |
| 반응물 | Ethyl (4-mercapto-2-methylphenoxy)acetate | HCID 16641178 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | Ethyl 2-(4-acetyl-2-methylphenoxy)acetate | HCID 21986544 | 159% |
반응 단계
To intermediate 4 (710 mg, 1.81 mmol) in DMF (50 mL) was added the K2CO3 (275 mg, 1.99 mmol) followed by the ethyl 2-bromo-2-methylpropanate (280 μL, 1.91 mmol; Aldrich) and the reaction heated to 80° C. After 18 h, the reaction cooled to rt and the solvent removed in vacuo. The residue treated with water (200 mL), extracted 3×50 mL CH2Cl2, dried over Na2SO4, filtered and the solvent removed under vaccum. The residue was chromatographed (CH2Cl2/MeOH: 99/1). To afford 680 mg (77%) of Intermediate 5 as a clear oil. 1H NMR(CDCl3): δ 7.95 (d, 2H), 7.60 (d, 2H), 7.15 (d, 2H), 6.75 (d, 2H), 6.05 (t, 1H), 4.45 (d, 2H), 4.15 (q, 2H), 2.65 (s, 3H), 1.50 (s, 6H), 1.20 (t, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07091237B2 |
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| 출처 데이터셋 | uspto-grants-2006_08 |
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| ORD ID | ord-ef292f5548cf455d9ca50f896ef61a98 |
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| 출처 메모 | uspto-grants-2006_08 |
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