関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | Benzyl-N-(1-cyanoethyl)glycine hydrochloride | HCID 68560147 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | Benzyl 2-[3,5-dichloro-2-methyl-6-oxo-1(6H)-pyrazinyl]acetate | HCID 10663926 | 55% |
反応手順
A stirred mixture of oxalyl chloride (5.3 mL, 60 mmol) and benzyl-N-(1-cyanoethyl)glycine hydrochloride (3.82 g, 15 mmol), as prepared in the preceding step, in 1,2-dichlorobenzene (30 mL) was heated to 100° C. overnight. The solvent was evaporated in vacuo and the residue was purified by flash column chromatography to give a solid. 10% Ethyl acetate in hexane (100 mL) was added and the solid was collected to give the title compound as an orange crystalline solid (2.7 g, 55%). 1H NMR (CDCl3) δ 7.38 (m, 5H), 5.24 (s, 2H), 4.89 (s, 2H), 2.34 (s,3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06476016B2 |
|---|
| 出典データセット | uspto-grants-2002_11 |
|---|
| ORD ID | ord-bdad4dda17044672b6408bb9714041a7 |
|---|
| 出典メモ | uspto-grants-2002_11 |
|---|