HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric acid magnesium salt (1:1) → HCID 53681393, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 13216467 | HCID 13216467 | — |
| Reactant | HCID 178418287 | HCID 178418287 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53681393 | HCID 53681393 | 55.4% |
Reaction Steps
A solution of 590 mg of the alcohol prepared in Example 13 in 75 ml of methylene chloride is combined with 271 mg of sodium acetate and 534 mg of pyridinium chlorochromate, and the mixture is stirred under argon for 50 minutes. The mixture is combined with a solution of 0.25 ml of isopropanol and 0.5 ml of pyridine in 50 ml of ether and further stirred for 10 minutes. Subsequently 7.5 g of magnesium sulfate is introduced, the reaction solution is filtered, and the residue is washed with ether. The organic solution is applied directly to a 30 g silica gel column and eluted with a hexane/8% acetone-hexane gradient, thus obtaining 325 mg of the title compound as an oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04532236 |
| Source dataset | uspto-grants-1985_07 |
| ORD ID | ord-d0eff45d19634e45a8947798d92f8e36 |
| Source note | uspto-grants-1985_07 |