Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Fluoroisatin | HCID 236566 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 2728520 | HCID 2728520 | — |
Reaction Steps
5-Fluoroisatin 32 (10 mmol, Lancaster, order no. 14553) was dissolved in acetone 46 (50 ml), K2CO3 (138 mg, 1 mmol) was added, and the mixture was stirred at room temperature for 5 hours. The course of the reaction was monitored by TLC (eluent: ethyl acetate). To work up the product the acetone was completely distilled off in vacuo. The residue was dissolved in ethyl acetate, and the solution was filtered over silica gel with ethyl acetate. The filtrate was concentrated to 20 ml, and hexane was added until precipitation started. To complete the precipitation, the solution was cooled to approx. 10° C. in a refrigerator overnight. The product which precipitated was filtered out with suction and dried in vacuo. The resulting crude product was recrystallized from ethyl acetate/hexane (1:4).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08124788B2 |
|---|
| Source dataset | uspto-grants-2012_02 |
|---|
| ORD ID | ord-0cc5eb7eb79140d4868715d20ae26da1 |
|---|
| Source note | uspto-grants-2012_02 |
|---|