HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium borohydride → 1-(4-Fluoro-phenyl)-2-methyl-1,4,5,6,7,8-hexahydro-2H-3-thia-2,4,5-triaza-phenanthrene 3,3-dioxide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | N-Methylsulfamoyl chloride | HCID 11789235 | — |
| Reactant | (8-Amino-quinolin-7-yl)-(4-fluoro-phenyl)-methanone | HCID 68183219 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 1-(4-Fluoro-phenyl)-2-methyl-1,4,5,6,7,8-hexahydro-2H-3-thia-2,4,5-triaza-phenanthrene 3,3-dioxide | HCID 68183432 | 2% |
Reaction Steps
N-methylsulfamoyl chloride 213 (729.9 mg, 5.63 mmol) was added to a solution of (8-amino-quinolin-7-yl)-(4-fluoro-phenyl)-methanone 367 (500 mg, 1.88 mmol) in pyridine (20 ml) and the mixture was stirred at room temperature for 18 h. NaBH4 (213 mg, 5.63 mmol) was added and stirring was continued at room temperature for 16 h. The reaction was quenched by the addition of water (20 ml) and the aqueous phase was extracted with EtOAc (30 ml). The organic phase was washed with brine (15 ml), dried (Na2SO4) and concentrated n vacuo. The crude residue was purified by column chromatography with heptane/EtOAc as the eluent to give the title compound (12 mg, 2%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09102688B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-9f1118930d7e4c528c4e85c3480d46cc |
| Source note | uspto-grants-2015_08 |