化工社化工社 化学情報印刷レポート · 研究参考用
Water → 3,3'-Benzene-1,4-diylbis(1-ethyl-1H-pyrazolo[4,3-b]pyridine)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,4-Benzenediboronic acid | HCID 230478 | — |
| 反応物 | 3-bromo-1-ethyl-1H-pyrazolo[4,3-b]pyridine | HCID 66727882 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water 1,2-dimethoxyethane | HCID 18180031 | — |
| 生成物 | 3,3'-Benzene-1,4-diylbis(1-ethyl-1H-pyrazolo[4,3-b]pyridine) | HCID 66728061 | 7.3% |
反応手順
A mixture of 1,4-phenylenediboronic acid (37.0 mg), 3-bromo-1-ethyl-1H-pyrazolo[4,3-b]pyridine (101 mg), Pd(PPh3)4 (25.8 mg) and Cs2CO3 (0.280 g) in DME/water (3/1, 4 mL) was exposed to microwave irradiation (120° C., 40 min), treated with water, and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt/hexane). Crystallization from AcOEt/hexane gave the title compound (6.00 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029536B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-860466cb5efe4e0b9b2a630d8f4ba9f7 |
| 出典メモ | uspto-grants-2015_05 |