HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 15231559, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Methoxy-4-nitrobenzenesulfonyl chloride | HCID 309458 | — |
| Reactant | HCID 15231558 | HCID 15231558 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 15231559 | HCID 15231559 | 64.4% |
Reaction Steps
600 mg of sodium hydride as a 60% dispersion in oil were added in portions, with stirring, to a solution of 3 g of 5-chloro-3-cycloheptyl-1,3-dihydro-2H- benzimidazol-2-one in 30 ml of THF. 3 g of 4-nitro-2- methoxybenzenesulfonyl chloride were then added and the reaction mixture was stirred for 18 hours. The reaction mixture was then poured into a water+ ice mixture, extracted with ethyl acetate and washed with water and the organic phase was dried over sodium sulfate and concentrated to dryness. 3.5 g of the expected product were obtained by crystallization from an iso ether/AcOEt mixture (60/40; v/v). M.p.=193° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05585394 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-17fa440da36142a9a4ba669c8ba156aa |
| Source note | uspto-grants-1996_12 |