HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium amide → 1,5-Dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium amide | HCID 24533 | — |
| Reactant | Methyl sulfate(1-) | HCID 4694097 | — |
| Reactant | 1-methyl 1,2,4,5-tetrahydro 2,4-diketo 3H-1,5-benzodiazepine | HCID 22749241 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | 1,5-Dimethyl-1H-1,5-benzodiazepine-2,4(3H,5H)-dione | HCID 536009 | — |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04001408 |
| Source dataset | uspto-grants-1977_01 |
| ORD ID | ord-60b7cf686da64f508159bc57b5ce7afc |
| Source note | uspto-grants-1977_01 |