関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-(4-Morpholinyl)acetohydrazide | HCID 351635 | — |
| 反応物 | Ethyl[2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate | HCID 76754608 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | HCID 178517484 | HCID 178517484 | — |
反応手順
1.33 g (4.7 mmol) of ethyl [2-cyano-1-(2,4-dichlorophenyl)ethenyl]carbamate (Example 128A) and 740 mg (4.7 mmol) of 2-morpholin-4-ylacetohydrazide are dissolved in NMP (6 ml) and stirred in a flask with a calcium chloride drying tube at an oil-bath temperature of 160° C. for 3 h. The reaction mixture is cooled to RT and ethyl acetate (100 ml) and water (50 ml) are added. The organic phase is separated off, dried with magnesium sulphate and concentrated. The residue is chromatographed on silica gel (mobile phase dichloromethane/methanol 100:1 to 50:1). 1.25 g (70% of theory) of the product are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09051323B2 |
|---|
| 出典データセット | uspto-grants-2015_06 |
|---|
| ORD ID | ord-6b0892285c6e47288621ff5cef23f71e |
|---|
| 出典メモ | uspto-grants-2015_06 |
|---|