HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 1,3-Dihydro-1-oxoisobenzofuran-5-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sulfamide | HCID 82267 | — |
| Reactant | 5-Chlorocarbonylphthalide | HCID 9815555 | — |
| Solvent | Sulfolane | HCID 31347 | — |
| Product | 1,3-Dihydro-1-oxoisobenzofuran-5-carbonitrile | HCID 821218 | — |
Reaction Conditions
| Temperature | 135 °C |
|---|
Reaction Steps
5-Chlorocarbonylphthalid (24.3 g, 0.124 mole) was dissolved in sulfolane (51 g). Sulfamide (13.8 g 0.144 mole) was added and the temperature was raised to 135° C. for 3 hours. At about 90° C., gas evolution took place. The mixture was allowed to cool and water (100 g) was added. The temperature was held at 85-90° C. for 5 min and then the solution was cooled to 60° C. The crystals were filtered off and washed with water (60 g) and acetic acid (30 g). Then the title compound was dried in vacuo. Yield: 19 g, 96%. Purity: 98.2% (hplc, peak area).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06441201B1 |
| Source dataset | uspto-grants-2002_08 |
| ORD ID | ord-04675e1251234481afd79f63b5410811 |
| Source note | uspto-grants-2002_08 |