関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Aminobenzonitrile | HCID 13396 | — |
| 反応物 | Heptafluorobutyryl Chloride | HCID 67810 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,2,3,3,4,4,4-heptafluoro-N-[4-(cyano)phenyl]butanamide | HCID 14253806 | 36.9% |
反応手順
A mixture of 4-aminobenzonitrile (1.58 g), triethylamine (1.36 g), and dichloromethane (20 mL) was cooled in ice under a nitrogen atmosphere. To this mixture was added perfluorobutyryl chloride (3.11 g) in dichloromethane (10 mL) and the resulting mixture was allowed to warm to room temperature and was then stirred for three hours. The reaction mixture was diluted with HCl solution (1N, 50 mL) and the layers were partitioned in a separatory funnel. The organic phase was washed with a saturated brine solution, dried over MgSO4, filtered and concentrated with a rotary evaporator. The residue was dissolved in dichloromethane. Upon dilution with hexane the product precipitated to give 1.55 g of 2,2,3,3,4,4,4-heptafluoro-N-[4-(cyano)phenyl]butanamide, m.p. 116°-118° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04764623 |
|---|
| 出典データセット | uspto-grants-1988_08 |
|---|
| ORD ID | ord-fd7a1f957094494980469d14f25061e8 |
|---|
| 出典メモ | uspto-grants-1988_08 |
|---|