化工社化工社 化学情報印刷レポート · 研究参考用
Acetonitrile → Ethyl cyanomethyl(1-(2-nitrophenyl)ethyl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-(1-(2-Nitrophenyl)ethylamino)acetonitrile | HCID 86625228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Ethyl cyanomethyl(1-(2-nitrophenyl)ethyl)carbamate | HCID 86625229 | 4% |
反応手順
To the acetonitrile solution containing 2-(1-(2-nitrophenyl)ethylamino)acetonitrile (18) from the previous step was added saturated NaHCO3 (5 mL) and ethyl chloroformate (1.83 g, 16.86 mmol). The reaction mixture was stirred vigorously at room temperature for 14 hours. The reaction was diluted with EtOAc (50 mL) and washed with brine (40 mL). The separated organic phase was dried over Na2SO4, filtered, and concentrated. Purification (Biotage 40 s, 3:1 CH2Cl2:hexanes, then 100% CH2Cl2) provided 37.1 mg (0.134 mmol, 4% yield) of ethyl cyanomethyl(1-(2-nitrophenyl)ethyl)carbamate (19) as a light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08163738B2 |
| 出典データセット | uspto-grants-2012_04 |
| ORD ID | ord-73031a8254104549b71c62d49b74bff1 |
| 出典メモ | uspto-grants-2012_04 |