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Water → 1-(2-Fluorobenzyl)-3-[5-(5-isopropyl-2,5-diazabicyclo[2.2.1]hept-2-yl)-2-pyrimidinyl]-1h-pyrazol[3,4-b]pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Isopropyl iodide | HCID 6362 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-[5-(2,5-Diazabicyclo[2.2.1]hept-2-yl)-2-pyrimidinyl]-1-(2-fluorobenzyl)-1h-pyrazolo[3,4-b]pyridine | HCID 21983517 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 1-(2-Fluorobenzyl)-3-[5-(5-isopropyl-2,5-diazabicyclo[2.2.1]hept-2-yl)-2-pyrimidinyl]-1h-pyrazol[3,4-b]pyridine | HCID 21983518 | — |
反応手順
50 mg (0.13 mmol) of 3-[5-(2,5-diazabicyclo[2.2.1]hept-2-yl)-2-pyrimidinyl]-1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridine (example 9) are dissolved in 5 ml of absolute acetone, and 92 mg (0.87 mmol) of sodium carbonate are added. 64 mg (0.37 mmol) of 2-iodopropane are added to the suspension, and the mixture is stirred at RT overnight. The reaction solution is mixed with water and extracted with DCM. The organic phases are combined, washed with saturated aqueous sodium chloride solution, dried and filtered. The solvent is removed in vacuo, and the residue is purified by preparative HPLC with addition of small portions of aqueous hydrochloric acid. 25 mg (42% of theory) of the product are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091198B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-3b9692a8f94a4325b9f1310600f39178 |
| 出典メモ | uspto-grants-2006_08 |