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Benzene → Ethyl 1,6-bis(1,1-dimethylethyl)-3-methyl-1H-pyrazolo[3,4-b]pyridine-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene | HCID 241 | — |
| 反応物 | Ethyl 5,5-dimethyl-2,4-dioxohexanoate | HCID 83403 | — |
| 反応物 | 1-tert-Butyl-3-methyl-1H-pyrazol-5-amine | HCID 737200 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Ethyl 1,6-bis(1,1-dimethylethyl)-3-methyl-1H-pyrazolo[3,4-b]pyridine-4-carboxylate | HCID 68081092 | — |
反応手順
The title compound was prepared in the same manner as described for intermediate 61 using ethyl 5,5-dimethyl-2,4-dioxohexanoate (392 mg, 1.958 mmol), benzene (10 mL), 1-(1,1-dimethylethyl)-3-methyl-1H-pyrazol-5-amine (300 mg, 1.958 mmol), and acetic acid (2 mL). The crude product was purified by column chromatography (Silica gel, eluent: 0 to 100% EtOAc/hexanes) to give 530 mg (85%) of product. LCMS E-S (M+H)=318.3. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.43-1.52 (m, 12H), 1.84 (s, 9H), 2.67 (s, 3H), 4.50 (q, J=7.07 Hz, 2H), 7.59 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08637509B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-040262c2b0be4256a7c5b9a3d0da0ef9 |
| 出典メモ | uspto-grants-2014_01 |