化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → Ethyl 5,6-Dichloronicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | 5,6-Dichloronicotinic acid | HCID 247987 | — |
| 生成物 | Ethyl 5,6-Dichloronicotinate | HCID 16762519 | — |
反応手順
To a solution of 5,6-dichloronicotinic acid (20.01 g, 104 mmol) in EtOH (500 mL) at 20° C. was added chlorotrimethylsilane (132 mL, 1042 mmol). The reaction was stirred for 72 hours. The reaction mixture was then concentrated and diluted with EtOAc (500 mL), and washed with saturated NaHCO3 (2×100 mL) and brine (100 mL). The organic was then dried (Na2SO4) and concentrated under reduced pressure to give final crude product (21.25 g). LCMS m/z 220.1 (M+H)+, Rt 0.94 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434719B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-5a45f9597fb941b9ae778f44080a3dfb |
| 出典メモ | uspto-grants-2016_09 |