HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → (+/-)-8-Methyl-5-(4-nitrophenyl)-7-(2-pyrimidinyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1-{6-[(4-Nitrophenyl)-(pyrimidin-2-yl-hydrazono)-methyl]-benzo-1,3-dioxol-5-yl}-propan-2-ol mesylate | HCID 131724742 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | (+/-)-8-Methyl-5-(4-nitrophenyl)-7-(2-pyrimidinyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine | HCID 22565487 | 77.5% |
Reaction Steps
A mixture of 3.13 g (6.27 mmol) of the compound obtained in Step B, 60 ml of a 1:1 mixture of dichloromethane-methanol and 0.52 ml (6.90 mmol) of 50% sodium hydroxide solution was stirred at room for 1.5 h. After filtration the reaction mixture was concentrated, the residue was treated with water and recrystallized from three fold dimethylformamide containing 10% water to yield 1.96 g (77%) of the title compound; Mp.: 261-263° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06858605B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-c641818e40aa43a2ac61a768a117d1fa |
| Source note | uspto-grants-2005_02 |