HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1979478Generated: October 30, 2026
Sodium Bicarbonate → HCID 21201956, compound
https://huagongshe.com/reaction/1979478
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 3-Bromocyclohept-1-ene | HCID 12453881 | — |
| Reactant | 3-Tert-butoxycarbonylamino-1,3,4,5-tetrahydrobenzo[b][1,4]diazepin-2-one | HCID 15490831 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21201956 | HCID 21201956 | 56.6% |
Reaction Steps
Sodium bicarbonate (1.6 g) and 3-bromocycloheptene (3.33 g) were added to a solution of 2-oxo-3-tert-butoxycarbonylamino-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (2.77 g) in N,N-dimethylformamide (20 ml), the mixture was stirred at 50° C. for one hour. After the reaction mixture was allowed to cool, ice-water was added thereto, extracted with ethyl acetate, the organic layer was washed with saturated brine. The resultant mixture was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography(ethyl acetate:n-hexane=1:2), diisopropyl ether was added to the residue for crystallization, and collected by filtration, to thereby obtain 2.1 g of the title compound as the mixture of diastereomer compounds.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06239131B1 |
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| Source dataset | uspto-grants-2001_05 |
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| ORD ID | ord-3943b9e952f14b899cd1cad78c1dfa5b |
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| Source note | uspto-grants-2001_05 |
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