HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methylcyclohexanone → HCID 58424286, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methylcyclohexanone | HCID 11567 | — |
| Reactant | Pyrrolidine | HCID 31268 | — |
| Reactant | 5'-Bromo-2'-hydroxyacetophenone | HCID 95991 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 58424286 | HCID 58424286 | 124.7% |
Reaction Steps
A mixture of 1-(5-bromo-2-hydroxy-phenyl)-ethanone (10 g, 46.7 mmol), 3-methylcyclohexanone (10.5 g, 93.4 mmol) and pyrrolidine (6.3 g, 88.8 mmol) in methanol (200 mL) was stirred overnight. The reaction mixture was concentrated in vacuo, and then H2O was added. The resulting solution was extracted with ethyl acetate. The organic layer was dried over anhydrous Na2SO4, filtered, and concentrated in vacuo to give 6-bromo-3′-methylspiro[chroman-2,1′-cyclohexan]-4-one (18 g, 100%). 1HNMR (CDCl3): 0.86 (m, 3H), 0.91 (m, 2H), 1.02 (m, 2H), 1.30 (m, 2H), 1.52 (m, 2H), 1.65 (m, 4H), 1.80 (m, 7H), 2.01 (m, 4H), 2.22 (m, 1H), 2.48 (m, 1H), 2.60 (s, 2H), 2.72 (t, 3H), 6.81 (m, 1H), 7.50 (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-f858aa86920d4a4f80ebe850132d6ddd |
| Source note | uspto-grants-2013_05 |