HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 19936399, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | 3-(4-Methoxy-benzyl)-3,4-diaza-bicyclo[4.1.0]heptan-2,5-dione | HCID 10776806 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 19936399 | HCID 19936399 | 29.6% |
Reaction Steps
To 5 ml of methylene chloride was added 462 mg (1.87 mmol) of (±)-3-(4-methoxybenzyl)-3,4-diazabicyclo[4.1.0]heptane-2,5-dione obtained in Reference Example 19. The mixture was cooled on a dry ice/ethanol bath, and 0.1 ml (1.1 mmol) of boron tribromide was added thereto dropwise. The temperature was elevated to room temperature, and the mixture was stirred for 2 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, the solvent was removed by distillation under reduced pressure, and the residue was recrystallized from ethanol/chloroform to obtain 120 mg (29.6%) of the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05418232 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-2154e15dceea4bc7b34faa003c458041 |
| Source note | uspto-grants-1995_05 |