HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium thiocyanate → (+/-)-8-Methyl-5-(4-nitrophenyl)-7-thiocarbamoyl-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium thiocyanate | HCID 516872 | — |
| Reactant | 1-(4-Nitrophenyl)-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine | HCID 10336422 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | (+/-)-8-Methyl-5-(4-nitrophenyl)-7-thiocarbamoyl-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine | HCID 12137394 | 76.1% |
Reaction Conditions
| Temperature | 105 °C |
|---|
Reaction Steps
A mixture of 0.90 g (9.26 mmol) of potassium thiocyanate, 2.00 g (6.15 mmol) of (±)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine and 40 ml of acetic acid was stirred at 100-110° C. for 6 h. After cooling, the precipitated crystals were filtered off, washed with water and dried to yield 1.80 g (76%) of the title compound. Mp.: 242-243° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06858605B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-58a86a71215a45fa83174b0b3f868e5d |
| Source note | uspto-grants-2005_02 |