HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,3-Dimethyl-1-(trifluoromethyl)-1,2-benziodoxole → HCID 86650728, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,3-Dimethyl-1-(trifluoromethyl)-1,2-benziodoxole | HCID 16043572 | — |
| Reactant | HCID 66602208 | HCID 66602208 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86650728 | HCID 86650728 | — |
Reaction Steps
Under argon, (4S)-4-(4-cyano-2-sulfanylphenyl)-3,6-dimethyl-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimidine-5-carbonitrile (45 mg, purity 50%, 53 μmol) was dissolved in dichloromethane (1 ml). At −78° C., 3,3-dimethyl-1-(trifluoromethyl)-1,3-dihydro-1λ3,2-benziodoxole (26 mg, 79 μmol; 1.5 eq.) was added, and the mixture was stirred for 2 h. The reaction solution was then concentrated under reduced pressure, and the residue was purified by preparative HPLC (Kromasil C18 column, 20×50 mm; mobile phase: acetonitrile/water+0.1% TFA). After lyophilization, the title compound was obtained as a solid (11.4 mg, 44% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09174997B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-fc2d9510f27a4137834013fa682317b9 |
| Source note | uspto-grants-2015_11 |