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Methanol → HCID 178471968、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Ethyl cyanoacetate | HCID 7764 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 9-oxo-9H-indeno(1,2-b)pyrazine-2,3-dicarbonitrile | HCID 292929 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178471968 | HCID 178471968 | 97.3% |
反応手順
Ethylcyanoacetate (110 mg, 0.970 mmol) was dissolved, under inert atmosphere, in dry DMF (1 ml) and NaH (39 mg, 0.970 mmol) was added in one portion. After 30 min, a solution of 1 (150 mg, 0.646 mmol) in dry DMF (2 ml) was added dropwise. After 15 min MeOH was added and the solution stirred for 10 min. The solvents were evaporated and the crude purified by flash chromatography (EtOAc:MeOH 9:1) affording 22 as a dark red solid (200 mg, 97%).
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-acdda630ff26422c8d67586bdcbc4117 |
| 出典メモ | uspto-grants-2014_02 |