HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 67753882, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 9928823 | HCID 9928823 | — |
| Product | HCID 67753882 | HCID 67753882 | 72% |
Reaction Steps
2 ml of thionyl chloride was added to 20 ml of methanol while cooling on ice, and then this solution was stirred at room temperature. 358 mg of the compound (30) obtained in Example 5 was added to the solvent, and the solution was heated at reflux for 8 hours. The solvent was removed and 40 ml of chloroform and 20 ml of water were added to the residue. The solution was alkalized with sodium hydrogen carbonate, and the organic layer was dried over magnesium sulfate. The solvent was removed by distillation. To the residue, ether was added and then ethyl acetate was added to form crystals. They were filtered off and washed with ethyl acetate in this order to obtain 270 mg of a title compound (121) (yield: 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05399553 |
| Source dataset | uspto-grants-1995_03 |
| ORD ID | ord-6ddcf7932f774586bb1940f30a32a178 |
| Source note | uspto-grants-1995_03 |