HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 15079735, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 12371433 | HCID 12371433 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 15079735 | HCID 15079735 | — |
Reaction Steps
To a solution of 14 g of 5-(2-chlorophenyl)-7-nitro-3H-1,4-benzodiazepine-2(1H)-thione (J. B. Hester, A. D. Rudzik & B. V. Kamdar, J. Med. Chem., 1971, 14, 1078-1081) in 700 ml of tetrahydrofuran were added firstly 260 ml of 25% aqueous ammonia solution and then 50 ml of methanol. The solution was stirred at room temperature for 20 h. and then concentrated to about 25 ml in a vacuum. The crystalline precipitate was filtered off and recrystallized from dioxan. There were obtained 13.2 g of 2-amino-5-(2-chlorophenyl)-7-nitro-3H-1,4-benzodiazepine of m.p. 222-224° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06174881B1 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-f0186301a3ac4ab9a4ed6c9998beb3d1 |
| Source note | uspto-grants-2001_01 |