HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 6-Fluoro-1,2,3,4-tetrahydroisoquinolin-1-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 5-Fluoro-1-indanone | HCID 136537 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 6-Fluoro-1,2,3,4-tetrahydroisoquinolin-1-one | HCID 10725709 | — |
Reaction Steps
Sodium azide (0.870 g, 13.33 mmol) was added in portions to a stirred solution of 5-fluoro-1-indanone (1.0 g, 6.67 mmol) and methanesulfonic acid (4 mL) in dichloromethane (4 mL) at 0° C. The reaction mixture was stirred at room temperature for 18 h. The mixture was then cooled to 0° C. and neutralized with 2N NaOH. The layers were separated, the aqueous layer extracted with dichloromethane, and the combined organic layers were dried over Na2SO4 and concentrated to give the title compound as a white powder. The crude product was used in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08993593B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-2235941ad5ed4dad8a3256aef7adacfd |
| Source note | uspto-grants-2015_03 |