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4-Amino-1-methylpiperidine → 4-(9-Cyclopentyl-7,7-difluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-ethyl-N-(1-methylpiperidin-4-yl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Amino-1-methylpiperidine | HCID 2737531 | — |
| 反応物 | Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 9886157 | — |
| 反応物 | 4-(9-cyclopentyl-7,7-difluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-ethylbenzoic acid | HCID 58015065 | — |
| 生成物 | 4-(9-Cyclopentyl-7,7-difluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-ethyl-N-(1-methylpiperidin-4-yl)benzamide | HCID 25253529 | — |
反応手順
The title compound was synthesized from 4-(9-cyclopentyl-7,7-difluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-ethylbenzoic acid as described in the General procedure for amide bond synthesis using HATU and 1-methylpiperidin-4-amine. The final compound was purified by reverse phase HPLC and basified to give the free base 1H NMR (400 MHz, DMSO-d6) δ ppm 1.14 (t, J=8.0 Hz, 3H) 1.23-1.69 (m, 11H) 1.77 (m, 4H) 1.99 (m, 2H) 2.20 (s, 3H) 2.69 (q, J=7.3 Hz, 2H) 3.75 (s, 1H) 3.97 (t, J=14.2 Hz, 2H) 4.54 (t, J=8.1 Hz, 1H) 7.57-7.81 (m, 3H) 8.12 (d, J=7.8 Hz, 1H) 8.17 (s, 1H) 8.61 (s, 1H). [M+H] calc'd for C28H37F2N7O2, 542. found 542.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08026234B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-75dd20128a5847afbce1d8cf0e94067a |
| 出典メモ | uspto-grants-2011_09 |