HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cornforth reagent → HCID 22119925, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cornforth reagent | HCID 2724130 | — |
| Reactant | HCID 22119976 | HCID 22119976 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22119925 | HCID 22119925 | 59.2% |
Reaction Steps
To a solution of 3-[3-(1-hydroxyethyl)-1,2-benzisothiazol-5-yl]-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione (3.99 g, 0.0107 mol) in dry methylene chloride under a nitrogen atmosphere is added powdered 4 Å molecular sieves followed by pyridinium dichromate (4.85 g, 0.0129 mol). The resultant mixture is stirred 22 hours at room temperature, diluted with ether, filtered through silica gel and diatomaceous earth, and concentrated in vacuo to a solid. The solid is recrystallized from ethyl acetate:hexanes to afford he title compound as a white crystalline solid (2.34 g, 59.2%, mp 149° C.) which is identified by NMR spectral analysis.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06156700 |
| Source dataset | uspto-grants-2000_12 |
| ORD ID | ord-23f628f74ce440c187e721c7aa482ddb |
| Source note | uspto-grants-2000_12 |