関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | (+/-)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbonitrile | HCID 12137416 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178421800 | HCID 178421800 | 101.7% |
反応手順
A mixture of 0.60 g (1.70 mmol) of the starting material XXIII, 3 ml of dimethylformamide, 0.12 g (1.87 mmol) of sodium azide and 0.10 g (1.87 mmol) of ammonium chloride was stirred at 140° C. for 30 min. The cooled reaction mixture was diluted with water and the precipitated crystals were filtered off. The so obtained product was purified by column chromatography using silica gel (MN Kieselgel 60) as adsorbent and a mixture of chloroform-methanol (99:1) as eluent to yield 0.68 g (54%) of the title compound; Mp.: 263-264° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06858605B2 |
|---|
| 出典データセット | uspto-grants-2005_02 |
|---|
| ORD ID | ord-2ca105df26b446e984445b4e84d6a6c2 |
|---|
| 出典メモ | uspto-grants-2005_02 |
|---|
