HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 2-oxo-3-tert-butoxycarbonylamino-5-(3-methyl-2-butenyl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Butene, 1-bromo-3-methyl- | HCID 70092 | — |
| Reactant | 2-oxo-3-tert-butoxycarbonylamino-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 21201581 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2-oxo-3-tert-butoxycarbonylamino-5-(3-methyl-2-butenyl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 21201744 | 75% |
Reaction Steps
2-Oxo-3-tert-butoxycarbonylamino-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (2.00 g) obtained from Referential Example 7 was suspended in methanol (20 ml), 1-bromo-3-methyl-2-butene (1.18 g) and potassium carbonate (997 mg) were added, the mixture was stirred for 2 hours at room temperature. The reaction mixture was concentrated under reduced pressure, water (100 ml) was added, and extracted with methylene chloride. The organic layer was washed with saturated aqueous sodium bicarbonate, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure, to thereby obtain 1.85 g of the titled compound (Yield: 71.4%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06239131B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-13fa98f2606243f2b4a762e4abc7a153 |
| Source note | uspto-grants-2001_05 |