関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphorus tribromide | HCID 24614 | — |
| 反応物 | HCID 178418997 | HCID 178418997 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,5-Dibromo-3-nitropyridine | HCID 298470 | 80.03% |
反応手順
To a solution of 5-Bromo-3-nitro-pyridin-2-ol (10.0 g, 45.66 mmol) in 70 ml of toluene and 7 ml of DMF was added PBr3 (6.60 ml, 68.49 mmol) and the reaction mixture was heated at 120° C. for 20 min under nitrogen atmosphere. After the completion of the reaction mixture (TLC monitoring), water (100 mL) was added and extracted with ethyl acetate (3×200 mL). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated to get the desired product (10.30 g, 80.03%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08088791B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-0836273d771b493b890fe97c749f6e1f |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|
