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Sodium amide → 1,5-Dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium amide | HCID 24533 | — |
| 反応物 | Methyl sulfate(1-) | HCID 4694097 | — |
| 反応物 | 1-methyl 1,2,4,5-tetrahydro 2,4-diketo 3H-1,5-benzodiazepine | HCID 22749241 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | 1,5-Dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione | HCID 536009 | — |
反応手順
2 g of sodium amide are added to a suspension of 9.5 g of 1-methyl 1,2,4,5-tetrahydro 2,4-diketo 3-H-1,5-benzodiazepine, obtained in the example XIV, in 30 c.c. of xylene, and the whole is heated for about thirty minutes, while agitating, treated with 20 c.c. of methyl-sulfate and as soon as the exothermic reaction has ceased, this is heated and boiled for three hours. The solvent is evaporated under reduced pressure, the residue is taken up in 200 c.c. of a 10% solution of caustic soda, and after agitation, suction filtered, and purified upon crystallisation in 90% ethanol. Yield 4.5 g; melting point : 240°-242° C. Analysis: C11H12N2O2Calculated: C % 64.69 H % 5.92; N % 13.72; Found: 64.67; 6.12; 13.95.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04001408 |
| 出典データセット | uspto-grants-1977_01 |
| ORD ID | ord-60b7cf686da64f508159bc57b5ce7afc |
| 出典メモ | uspto-grants-1977_01 |