HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron tribromide → HCID 19595300, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron tribromide | HCID 25134 | — |
| Reactant | HCID 19595141 | HCID 19595141 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 19595300 | HCID 19595300 | 17% |
Reaction Steps
Boron tribromide (8.8 g) was added dropwise to a solution of 6-fluoro-7-methoxy-2-(4-pyridinylamino)-1,2,3,4-tetrahydroisoquinoline (2.9 g) in dichloromethane (200 mL) at -78° C. The dry ice bath was removed, and the suspension was stirred at ambient temperature for 3 hrs. The reaction mixture was cooled to -78° C., and methanol (100 mL) was added. The mixture was stirred at ambient temperature for 1 hr and concentrated in vacuo. The residue was washed with methanol/ethyl ether and recrystallized from 2-propanol/ethyl acetate to give 0.61 g (17%) of product, mp 244-245° C. (dec).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06004977 |
| Source dataset | uspto-grants-1999_12 |
| ORD ID | ord-6b5bd79ca8b543018d8dfc7005c109a2 |
| Source note | uspto-grants-1999_12 |