HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 18989191, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | HCID 18989178 | HCID 18989178 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 18989191 | HCID 18989191 | 84.6% |
Reaction Steps
A solution of 4-(3-cyclopropyl-2-t-butyloxycarbonyl-1,3-dioxoprop-1-yl)-2,2-difluoro-7-methylsulphenyl-1,3-benzodioxole (10.3 g) and para-toluenesulphonic acid (0.5 g) was heated under reflux with toluene for 3 hours. After cooling, the solvent was evaporated in vacuo, and ethyl acetate added. The solution was washed with water, dried over anhydrous magnesium sulphate and evaporated. The residue was purified by column chromatography, eluting with ethyl acetate/cyclohexane to yield 4-(3-cyclopropyl-1,3-dioxoprop-1-yl)-2,2-difluoro-7-methylsulphenyl-1,3-benzodioxole (6.61 g) m.p. 117.5°-118.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05489570 |
| Source dataset | uspto-grants-1996_02 |
| ORD ID | ord-77eb080df34740a0a639bb4147170670 |
| Source note | uspto-grants-1996_02 |