関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Methyl chloroglyoxylate | HCID 79846 | — |
| 反応物 | 1-(4-Chloro-2-phenylamino-phenyl)-propan-1-one | HCID 70816614 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl (n-(5-chloro-2-propionylphenyl)-N-phenylcarbamoyl)formate | HCID 70816656 | 87.6% |
反応手順
To a solution of 1-(4-chloro-2-phenylamino-phenyl)-propan-1-one (13.0 g, 50.2 mmol) in toluene (150 mL) was added methyl chlorooxoacetate (42.86 g, 350.0 mmol) at room temperature under nitrogen. The reaction mixture was heated at reflux at 110° C. for 16 hr. Completion of the reaction was monitored by silica TLC (mobile phase; hexane:ethyl acetate=1:1; Rf=0.5). The reaction mixture was concentrated under vacuum to afford 15.2 g (87.6% crude yield) of N-(5-chloro-2-propionyl-phenyl)-N-phenyl-oxalamic acid methyl ester. The crude product was used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08501732B2 |
|---|
| 出典データセット | uspto-grants-2013_08 |
|---|
| ORD ID | ord-d8fb32f5730d4ecaa7e2e137302bf31b |
|---|
| 出典メモ | uspto-grants-2013_08 |
|---|