HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 19917712, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Tert-butyl-7-chloro-1,3-dihydro-1,4-benzodiazepine-2,5-dione | HCID 178104 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 19917712 | HCID 19917712 | 118.1% |
Reaction Steps
Methyl iodide (233 μL, 3.7 mmol) is added to a mixture of 7-chloro-4-tert-butyl-3,4-dihydro-1H-1,4-benzodiazepine-2,5-dione (0.5 g, 1.9 mmol) and potassium carbonate (1.04 g, 7.5 mmol) in tetrahydrofuran. The reaction mixture is stirred at room temperature for 16 hours, heated at reflux for 90 hours, filtered through diatomaceous earth and concentrated in vacuo to obtain a residue. Flash column chromatography of the residue using silica gel and 33% to 50% ethyl acetate in hexanes solutions gives the title product as a clear oil (0.63 g) which is identified by 1HNMR spectral analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05438035 |
| Source dataset | uspto-grants-1995_08 |
| ORD ID | ord-b8300315a37f4eb684b4f7db31e9ce65 |
| Source note | uspto-grants-1995_08 |