関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | (R)-(+)-4-(Chloromethyl)-2,2-dimethyl-1,3-dioxolane | HCID 2734443 | — |
| 反応物 | HCID 178506553 | HCID 178506553 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Acetonitrile--water (1/1) | HCID 18373917 | — |
| 生成物 | HCID 67469660 | HCID 67469660 | 34.8% |
反応手順
7-Iodo-2H-pyrazolo[4,3-b]pyridine (100 mg, 0.408 mmol), (R)-4-(chloromethyl)-2,2-dimethyl-1,3-dioxolane (0.056 ml, 0.408 mmol) and cesium carbonate (266 mg, 0.816 mmol) were combined in DMF (5 mL) at room temperature. The mixture was heated at 120° C. for 1 hour, then cooled and purified by preparative HPLC using a Phenomenex Gemini Prep 5 μm C18, 75×30 mm column eluting with a gradient of 20-70% 10 mmol NH4HCO3 in 20/80 (v/v) water/acetonitrile in 10 mmol NH4HCO3 in water to give (S)-2-((2,2-dimethyl-1,3-dioxolan-4-yl)methyl)-7-iodo-2H-pyrazolo[4,3-b]pyridine (51 mg, 34.8% yield). MP 85-87° C. MS [M+H] found 360.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09073918B2 |
|---|
| 出典データセット | uspto-grants-2015_07 |
|---|
| ORD ID | ord-e2f63fd7ee0d4a1598849b8413c228fe |
|---|
| 出典メモ | uspto-grants-2015_07 |
|---|
