関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 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 | Diethyl 4-(amino(phenyl)methyl)phenylphosphonate | HCID 89462707 | — |
| 反応物 | HCID 178524762 | HCID 178524762 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178476968 | HCID 178476968 | — |
反応手順
To a solution of 4-hydroxy-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylic acid, 8-b, (309 mg, 1.5 mmol) in MeCN (10 ml) were added HATU (599 mg, 1.58 mmol), Et3N (159 mg, 1.58 mmol) and diethyl 4-(amino(phenyl)methyl)phenylphosphonate, 2-c, (479 mg, 1.5 mmol). The resulting mixture was stirred at room temperature for 2 hours. Then it was concentrated under vacuum and the residue was taken into ethyl acetate followed by washing with sat. NH4Cl. The organic layer was dried over sodium sulfate and concentrated under vacuum. The residue was purified by prep-HPLC to provide the product, 8-1, (150 mg, 20%). 1H NMR (CD3OD, 300 MHz,): δ 10.39 (br, 1H), 8.56 (s, 1H), 8.47 (m, 1H), 7.81 (m, 1H), 7.62 (m, 2H), 7.40 (m, 2H), 7.25 (m, 5H), 6.54 (m, 1H), 6.26 (m, 1H), 3.96 (m, 4H), 1.18 (m, 6H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09079930B2 |
|---|
| 出典データセット | uspto-grants-2015_07 |
|---|
| ORD ID | ord-7ad4f8e4765e4b588fd23f8145b8b77f |
|---|
| 出典メモ | uspto-grants-2015_07 |
|---|
