HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorodifluoromethane → HCID 18696206, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorodifluoromethane | HCID 6372 | — |
| Reactant | Sodium Methoxide | HCID 10942334 | — |
| Reactant | HCID 18696107 | HCID 18696107 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18696206 | HCID 18696206 | 16% |
Reaction Steps
To a solution of 5-hydroxy-3-(2-(N-t-butoxycarbonylamino)ethoxy)-1,2-benzisoxazole (100 mg) in dimethylformamide (4 ml) was added sodium methoxide (90 mg) and the mixture was stirred at room temperature for 10 minutes, then followed by introduction of chlorodifluoromethane gas for 20 minutes. The reaction mixture was poured into ice water (30 ml), extracted with ethyl acetate (twice each with 30 ml) and the combined extracted were dried over anhydrous magnesium sulphate and filtered. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography with cyclohexane/ethyl acetate (9/1) as an eluent, to give the title compound (19 mg, 16%) as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06096771 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-1fcc8556b5aa4f929ac0e011fef47347 |
| Source note | uspto-grants-2000_08 |