참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Sodium Azide | HCID 33557 | — |
| 반응물 | (+/-)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbonitrile | HCID 12137416 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | HCID 178421800 | HCID 178421800 | 101.7% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06858605B2 |
|---|
| 출처 데이터셋 | uspto-grants-2005_02 |
|---|
| ORD ID | ord-2ca105df26b446e984445b4e84d6a6c2 |
|---|
| 출처 메모 | uspto-grants-2005_02 |
|---|
