HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 23222722, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | HCID 15295198 | HCID 15295198 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 23222722 | HCID 23222722 | 98.2% |
Reaction Steps
A mixture of 4-cyano-4-(3,4-bisdifluoromethoxyphenyl)cyclohexan-1-one (1.34 g, 4.05 mmol), trimethyl orthoformate (0.53 mL, 4.85 mmol) and a catalytic amount of p-toluenesulfonic acid in methanol (40 mL) was heated gently under an argon atmosphere for 2 h. The mixture was cooled and then concentrated The residue was partitioned between 5% aqueous sodium carbonate and ethyl acetate, was extracted twice with ethyl acetate, the organic extract was dried (potassium carbonate) and the solvent was removed in vacuo to provide an oil (1.5 g, 98%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05811455 |
| Source dataset | uspto-grants-1998_09 |
| ORD ID | ord-67982fce6eae486cae6125f820d057ac |
| Source note | uspto-grants-1998_09 |