HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Hydroxide → NSC245059
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Oxalic acid dihydrate | HCID 61373 | — |
| Reactant | 1,2,3,4,4a,5,8,8a-Octahydro-1,4:5,8-dimethanonaphthalen-2-yl acetate | HCID 269443 | — |
| Solvent | Water | HCID 962 | — |
| Product | NSC245059 | HCID 428925 | 95% |
Reaction Steps
100 parts of 8-acetoxytetracyclo[4.4.0.12,5.17,10]dodec-3-ene, 200 parts of 1,4-dioxane, 50 parts of distilled water, and 50 parts of potassium hydroxide were placed in a flask. A hydrolysis reaction was carried out for 4 hours in a nitrogen atmosphere at 100° C. After cooling, an aqueous solution of oxalic acid di-hydrate in an amount of 1.1 equivalent of the potassium hydroxide was added dropwise to coagulate the reaction product. The coagulate was washed with a large amount of water, then washed with a small amount of toluene, and dried to obtain 8-hydroxytetracyclo [4.4.0.12,5.17,10]dodec-3-ene of the following formula (14) at an yield of 95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06180316B2 |
| Source dataset | uspto-grants-2001_01 |
| ORD ID | ord-22d0014651f947c4a34c59419dedbfa1 |
| Source note | uspto-grants-2001_01 |