化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → cyano-(2-cyano-9-oxo-9H-indeno[1,2-b]pyrazin-3-yl)-acetic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | tert-Butyl cyanoacetate | HCID 70693 | — |
| 反応物 | 9-oxo-9H-indeno(1,2-b)pyrazine-2,3-dicarbonitrile | HCID 292929 | — |
| 生成物 | cyano-(2-cyano-9-oxo-9H-indeno[1,2-b]pyrazin-3-yl)-acetic acid tert-butyl ester | HCID 67059687 | — |
反応手順
tert-Butyl cyanoacetate (292 mg, 2.07 mmol) was dissolved, under inert atmosphere, in dry DMF (4 ml) and NaH (60% dispersion in mineral oil, 90 mg, 2.24 mmol) was added portionwise. After 15 min, a solution of 1 (400 mg, 1.72 mmol) in dry DMF (3 ml) was added dropwise. After 16 h MeOH was added, the solvents were evaporated and the crude purified by flash chromatography (EtOAc:MeOH 9:1) affording cyano-(2-cyano-9-oxo-9H-indeno[1,2-b]pyrazin-3-yl)-acetic acid tert-butyl ester as dark red solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08648076B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-f5102584cb404712985212225415f4f6 |
| 出典メモ | uspto-grants-2014_02 |