HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 53936706, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 53874904 | HCID 53874904 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53936706 | HCID 53936706 | 74.3% |
Reaction Steps
350 mg of 2-[1-(5-cyano-2-hydroxyphenyl)-3-methyl-2butenyl]-6-methylpyridine N-oxide in 15 ml of dichloromethane were stirred with 100 μl of concentrated sulphuric acid for 1 hour. A further 100 μl of concentrated sulphuric acid were added and stirring was continued for 30 minutes. The mixture was washed with water, dried over sodium sulphate and evaporated. The residue was chromatographed on silica gel using methanol/ethyl acetate (1:9) for the elution to give an oil which crystallized from diethyl ether. There was obtained 0.26 g of 2-(6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-4-yl)-6-methylpyridine N-oxide of melting point 165-167° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05118694 |
| Source dataset | uspto-grants-1992_06 |
| ORD ID | ord-c23e85f05e904562845ac52e9b946163 |
| Source note | uspto-grants-1992_06 |