HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 67427979, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Ethyl Glycolate | HCID 12184 | — |
| Reactant | 2,5-Difluorobenzonitrile | HCID 123558 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 67427979 | HCID 67427979 | 21% |
Reaction Steps
To a solution of 2,5-difluoro-benzonitrile (10 g, 72.0 mmol) in DMF (200 mL) was added hydroxy-acetic acid ethyl ester (8.6 mL, 86.4 mmol) followed by K2CO3 (43.7 g, 316 mmol). After 24 h at 100° C., the reaction mixture was diluted with 1 N NaOH (200 mL) and extracted with CH2Cl2 (3×150 mL). The combined organic layers were washed with 1 N NaOH (100 mL), dried, and concentrated to afford the desired product (3.35 g, 21%). 1H NMR (CDCl3): 7.39 (dd, J=9.0, 4.0 Hz, 1H), 7.21-7.15 (m, 2H), 4.90 (s, 2H), 4.45 (q, J=7.1 Hz, 2H), 1.47 (t, J=7.1 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030321B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-0af9019c9dc5494b9e15e6f91be6831b |
| Source note | uspto-grants-2011_10 |