Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | HCID 18183110 | HCID 18183110 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 18183175 | HCID 18183175 | 172.8% |
Reaction Steps
4.3 g of 8-methoxy-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepin-4-one is mixed in 48 ml of pyridine with 2.46 g of diphosphorus pentasulfide and stirred under argon and with exclusion of moisture for 2 hours at a bath temperature of 100° C. It is diluted with water, and the precipitated product is suctioned off. After chromatography on silica gel first with ethyl acetate:hexane=1:1 and later with ethyl acetate, a total of 3.13 g of 8-methoxy-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine-4-thione is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06323197B1 |
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| Source dataset | uspto-grants-2001_11 |
|---|
| ORD ID | ord-c15507d17fa34ef098924cfe730fc7d7 |
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| Source note | uspto-grants-2001_11 |
|---|
