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Diisopropylethylamine → HCID 44242929、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | phenyl 3-tert-butyl-1-methyl-1H-pyrazol-5-ylcarbamate | HCID 46196890 | — |
| 反応物 | 3-(6-Methoxy-7-(2-methoxyethoxy)quinazolin-4-yloxy)aniline | HCID 66875805 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 生成物 | HCID 44242929 | HCID 44242929 | — |
反応手順
The procedure in 138B was used to react the carbamate from Example 157A (123 mg, 0.45 mmol) with 3-(6-methoxy-7-(2-methoxyethoxy)quinazolin-4-yloxy)aniline from Example 117B (103 mg, 0.30 mmol). To this solution was added diisopropylethyl amine (78 μL, 0.45 mmol) and DMAP (3.6 mg, 0.03 mmol). The reaction was concentrated to dryness. The resulting oil purified by silica gel chromatography eluting with ethyl acetate/dichloromethane 10-50% over 60 minutes. The main peak concentrated to a solid weighing 126 mg. 1H (DMSO-d6) 9.10 (s, 1H), 8.70 (s, 2H), 7.65 (m, 2H), 7.50 (m, 2H), 7.30 (m, 1H), 7.15 (s, 1H), 6.95 (m, 1H), 6.00 (s, 1H), 4.40 (s, 2H), 4.00 (s, 3H), 3.85 (s, 2H), 3.60 (s, 3H), 3.40 (s, 3H), 1.25 (s, 9H). LCMS (ESI) m/z 521 (M+H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08969587B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-8b1c26db32164cb9998f21dd34ee6e75 |
| 出典メモ | uspto-grants-2015_03 |