HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21201828, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 3,3-Dimethylbutanoyl chloride | HCID 81514 | — |
| Reactant | 2-oxo-3-tert-butoxycarbonylamino-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine | HCID 21201581 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 21201828 | HCID 21201828 | 94.6% |
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 1,2-dichloroethane (40 ml), 3,3-dimethylbutanoyl chloride (1.07 g) and pyridine (627 mg) were added, and the mixture was refluxed for 2 hours. Water was added to the reaction mixture, separated, 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 2.53 g of the titled compound (Yield: 90.1%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06239131B1 |
| Source dataset | uspto-grants-2001_05 |
| ORD ID | ord-30db1f16a00a4e90bda3c1c467b817d6 |
| Source note | uspto-grants-2001_05 |