Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Pyridazinecarbonitrile, 2,3-dihydro-3-oxo-5,6-diphenyl- | HCID 95757 | — |
| Reactant | 2-Bromoethanesulfonic acid, sodium salt | HCID 23666797 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 13533510 | HCID 13533510 | 50.1% |
Reaction Steps
7.5 grams (0.027 mole) of the product of Example 1 was caused to react with 3.79 grams of K2CO3 in the least amount of water along with 200 mls of DMF. To this mixture was added 5 drops of 18 crown-6-ether. Into this solution was added 5.79 grams (0.027 mole) of 2-bromoethane sulfonic acid sodium salt and the mixture heated to 110° C. for 3 hours. The solution was filtered and the filtrate was distilled at reduced pressure. The residual solid was dissolved in excess water and poured into conc. hydrochloric acid. The solid that precipitated was filtered and washed with water and then air dried. The recovered solid was recrystallized from acetonitrile to give 2.7 grams of a yellow solid which melted at 138°-140° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04545810 |
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| Source dataset | uspto-grants-1985_10 |
|---|
| ORD ID | ord-66ac0158d8074536b9b18328140f45bc |
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| Source note | uspto-grants-1985_10 |
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