HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 13826776, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methyl dichloroacetate | HCID 8315 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 105679-42-3 | HCID 135589616 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 13826776 | HCID 13826776 | 55.3% |
Reaction Steps
A mixture of 5,6-dihydroxy-3-phenyl-1,2-benzisoxazole (2.9 g), potassium carbonate (10.7 g) and methyl dichloroacetate (3.7 g) in 50 ml of N,N-dimethylformamide was stirred at 90°-100° C. for 2.5 hours. After cooling, water (50 ml) was added to the mixture followed by stirring it at 90°-100° C. for 40 minutes. After cooling and acidifying the mixture with hydrochloric acid, the mixture was extracted with ether. The ether layer was washed with water, dried and evaporated to remove the solvent. The residue was washed with methylene chloride, recrystallized from acetone/water to give 2.0 g of 3-phenyl-1,3-dioxolo[4,5-f]-1,2-benzisoxazole-6-carboxylic acid. m.p.: 202.5°-203.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04732906 |
| Source dataset | uspto-grants-1988_03 |
| ORD ID | ord-f1d6be5924114c9091a4085c812bb2be |
| Source note | uspto-grants-1988_03 |