Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Sodium Bisulfate | HCID 516919 | — |
| Reactant | HCID 13055586 | HCID 13055586 | — |
| Catalyst | chromium (VI) trioxide | HCID 10219390 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 13055588 | HCID 13055588 | 76.6% |
Reaction Steps
Under an atmosphere of nitrogen, 100 mg of chromium trioxide and 0.5 g of infusorial earth were added to 0.162 ml of pyridine in 3 ml of methylene chloride, and the mixture was stirred for 15 minutes at room temperature. 55 mg of the 3-hydroxy compound (prepared as described in Example 1) in 1 ml of methylene chloride were added thereto at 0° C., and the mixture was stirred for 20 minutes at the same temperature. To the reaction solution obtained was added 1 g of sodium bisulphate and, after stirring for 20 minutes at 0° C., the mixture was filtered through a magnesium sulphate layer. The filtrate was concentrated under reduced pressure. The residue obtained was purified by column chromatography on silica gel using a mixture of cyclohexane and ethyl acetate (6:1) as eluent to obtain 42 mg of the title compound having the following physical characteristics:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04351846 |
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| Source dataset | uspto-grants-1982_09 |
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| ORD ID | ord-425a02627e1041e9bde79ea5a2621a06 |
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| Source note | uspto-grants-1982_09 |
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