化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl Acetate → (R)-2-(3-bromo-4-cyanophenylamino)propanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Dimethylacetamide | HCID 31374 | — |
| 反応物 | 2-Bromo-4-fluorobenzonitrile | HCID 118939 | — |
| 反応物 | (2R)-2-Aminopropanamide hydrochloride | HCID 2775814 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (R)-2-(3-bromo-4-cyanophenylamino)propanamide | HCID 67509792 | 69% |
反応手順
A solution of 2-bromo-4-fluorobenzonitrile (200 mg, 1.00 mmol), D-alanine amide hydrochloride (148 mg, 1.19 mmol) and DMA (0.620 mL, 3.56 mmol) in DMSO (3 mL) was stirred at 100 C for 18 h. EtOAc and water were added. The organic phase was separated, dried over Na2SO4, concentrated in vacuo. The residue was purified by a silica gel column, eluted first with 30% EtOAc in hexane, then with 100% EtOAc to give (R)-2-(3-bromo-4-cyanophenylamino)propanamide (185 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846928B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b944b628013f4510976ce132dfb416ca |
| 出典メモ | uspto-grants-2014_09 |