HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroborane-methyl sulfide → 4-[3-bromo-2-(3,5-dimethylisoxazol-4-yl)-1H-indole-1-yl]phenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroborane-methyl sulfide | HCID 11137191 | — |
| Reactant | 4-(3-bromo-1-(4-methoxyphenyl)-1H-indol-2-yl)-3,5-dimethylisoxazole | HCID 58378224 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 4-[3-bromo-2-(3,5-dimethylisoxazol-4-yl)-1H-indole-1-yl]phenol | HCID 44466357 | — |
Reaction Steps
At 0° C., 10 eq of boron trifluoride-dimethyl sulfide was added to 4-[3-bromo-1-(4-methoxyphenyl)-1H-indol-2-yl]-3,5-dimethylisoxazole (the intermediate product of step (b) from the synthesis of Example 22), dissolved in DCM and stirred at ambient temperature over night. The mixture was diluted with EtOAc and washed with brine, the organic phase was concentrated and subjected to reversed phase preparative HPLC. Appropriate fractions were combined and evaporated, and identified by ES/MS m/z: 385.1 (M+H), 383.09 (M−H) and 1H NMR (acetone-d6, 500 MHz): 7.60 (m, 1H), 7.31-7.23 (m, 3H), 7.17 (m, 2H), 6.95 (m, 2H), 2.28 (s, 3H) and 1.99 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08367665B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-a95d80f98f504af5901f5b9334b33f8d |
| Source note | uspto-grants-2013_02 |