HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 6-Bromospiro[2H-1-benzopyran-2,1′-cyclopentan]-4(3H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Cyclopentanone | HCID 8452 | — |
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 5'-Bromo-2'-hydroxyacetophenone | HCID 95991 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | 6-Bromospiro[2H-1-benzopyran-2,1′-cyclopentan]-4(3H)-one | HCID 59167871 | 110.9% |
Reaction Steps
A mixture of 1-(5-bromo-2-hydroxy-phenyl)-ethanone (15.8 g, 73.8 mmol), cyclopentanone (12.35 g, 147 mmol) and pyrrolidine (12 mL, 140 mmol) in MeOH (300 mL) was stirred at room temperature overnight. The mixture was concentrated in vacuo to give the residue, which was added water and HCl (36%) until pH=1. The mixture was extracted with EtOAc and then the organic layer was concentrated to give 6-bromospiro[chroman-2,1′-cyclopentan]-4-one (23 g, 100%). 1H-NMR (CDCl3): 1.64 (m, 4H), 1.72 (m, 2H), 2.03 (m, 2H), 2.78 (s, 2H), 6.78 (m, 1H), 7.48 (m, 1H), 7.91 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450308B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-d65905df40ea4b188b4a8fca46baaa0b |
| Source note | uspto-grants-2013_05 |