HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 21138134, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Cyclopentyl 4-methylbenzene-1-sulfonate | HCID 317685 | — |
| Reactant | HCID 88111276 | HCID 88111276 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21138134 | HCID 21138134 | 77.8% |
Reaction Steps
1 g of the product prepared in Example 31, 8.7 cm3 of dimethylformamide and 82 mg of sodium hydride are agitated for 30 minutes. Then 486 mg of cyclopentyl 4-methylbenzenesulphonate is added, agitation is carried out for 5 hours, the whole is poured into an aqueous solution of ammonium chloride, extracted with ethyl acetate, washed with salt water, dried and the solvent is evaporated off. The residue is chromatographed on silica (eluant: methylene chloride-isopropanol 95-5) and 861 mg of product is obtained which is crystallized from a methylene chloride/ethyl ether mixture and 777 mg of expected product is collected.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06596885B2 |
| Source dataset | uspto-grants-2003_07 |
| ORD ID | ord-f8ebb8b9fe80406eaa0da6eed7af091b |
| Source note | uspto-grants-2003_07 |