関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Acetophenone | HCID 7410 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Glyoxylic acid, monohydrate | HCID 15620607 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Phenyl-6-pyridazone | HCID 75106 | — |
反応手順
19.6 g (162.95 mmol) of 1-phenylethanone and 5 g (54.32 mmol) of oxoacetate monohydrate were stirred at 100° C. for 2 hours. The reaction solution was then cooled to 40° C., and 20 ml of water and 4 ml of ammonia were added. The mixture was then twice extracted with 50 ml of dichloromethane. 2.64 ml (53.32 mmol) of hydrazine monohydrate were then added to the aqueous phase obtained, and the mixture was stirred at 100° C. for 2 hours. After the reaction, the reaction solution was cooled to room temperature. The precipitated crystals were filtered off with suction, washed with water and dried in a vacuum drying cabinet at 50° C. overnight. This gave 4.3 g (24.97 mmol, 15% of theory) of the title compound as colorless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08987256B2 |
|---|
| 出典データセット | uspto-grants-2015_03 |
|---|
| ORD ID | ord-7abf0e199c0a420bbf6b4612125e53d1 |
|---|
| 出典メモ | uspto-grants-2015_03 |
|---|