関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Cyclohexanecarbohydrazide | HCID 240039 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2H-1,5-Benzodiazepin-2-one, 4-ethoxy-1,3-dihydro- | HCID 58957915 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-cyclohexyl-4H,6H-2,3,6,10b-tetraaza-benzo[e]azulen-5-one | HCID 58957932 | — |
反応手順
To a solution of 4-ethoxy-1,3-dihydro-benzo[b][1,4]diazepin-2-one (Preparation 3(A) (5 g, 24.5 mmol) in glacial acetic acid (75 mL) was added cyclohexanecarboxylic acid hydrazide (Preparation 14) (3.5 g, 24.5 mmol). The reaction was heated at 120° C. for 2.5 hours, was cooled to room temperature, and EtOAc (50 mL), water (50 mL) and aqueous NaHCO3 (50 mL) were added. The mixture was stirred for 5 minutes and Et2O was added (125 mL). The suspension was stirred for 15 minutes and the solids were removed by filtration with the aid of Et2O to provide 5.92 g of 1-cyclohexyl-4H,6H-2,3,6,10b-tetraaza-benzo[e]azulen-5-one.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07265104B2 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-9aba5b85b52e4d65a8a109a030e7cf10 |
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| 出典メモ | uspto-grants-2007_09 |
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