関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetoacetate | HCID 8868 | — |
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 反応物 | Acetic Acid N'-(3,4-Dichlorophenyl)hydrazide | HCID 612829 | — |
| 生成物 | HCID 178429550 | HCID 178429550 | 41.3% |
反応手順
To a mixture of (V) (5.0 g, 22.8 mmol) and ethyl acetoacetate (2.97 g 22.8 mmol) was slowly added PCl3 (3.13 g, 22.8 mmol). The mixture was warmed to 50° C. for 1.5 h, poured into ice water (150 ml), and the resulting precipitate was collected on a sintered glass funnel and recrystallized from EtOH to yield (VI) (2.29 g, 41%) as white crystals, mp 208-211° C. (lit. 208-209° C.), TLC CHCl3/MeOH 9:1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08202872B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-982b049c4fbe44d9a01de70be49f90a2 |
|---|
| 出典メモ | uspto-grants-2012_06 |
|---|
