HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hexamethyldisilazide → 3-(2-Fluoro-4-iodophenyl)-1-(cyclopropylsulfonyl)-4-fluoro-8-methyl-1H-imidazo[4,5-g]quinazolin-2(3H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Reactant | Cyclopropanesulfonyl chloride | HCID 2760919 | — |
| Reactant | 3-(2-Fluoro-4-iodophenyl)-4-fluoro-8-methyl-1H-imidazo[4,5-g]quinazolin-2(3H)-one | HCID 59519492 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-(2-Fluoro-4-iodophenyl)-1-(cyclopropylsulfonyl)-4-fluoro-8-methyl-1H-imidazo[4,5-g]quinazolin-2(3H)-one | HCID 59519445 | 75% |
Reaction Conditions
| Temperature | -78 °C |
|---|
Reaction Steps
To a solution of 3-(2-fluoro-4-iodophenyl)-4-fluoro-8-methyl-1H-imidazo[4,5-g]quinazolin-2(3H)-one (50 mg, 0.12 mmol) in THF (10 ml) at −78° C. was added LiHMDS (0.16 ml, 1 M in THF, 0.16 mmol). The reaction mixture was stirred at −78° C. for 10 min and cyclopropylsulfonyl chloride (25 mg, 0.18 mmol) was added to the mixture. The reaction was slowly warmed to room temperature and stirred at the temperature for 16 h. The reaction was quenched with saturated aqueous NH4Cl solution (10 ml) and extracted with EtOAc (2×10 ml). The combined organic solution was washed with brine (20 ml), dried over MgSO4 and concentrated. Silica gel chromatography (EtOAc:Hexanes=25:75) yields 46 mg (75%) of the title compound as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07820664B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-da177f97aeb74a22a767056963d8ef9d |
| Source note | uspto-grants-2010_10 |