HuagongsheHuagongshe Chemistry Print Report · For research reference only
Urea → 2-Bromo-4-chlorobenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Urea | HCID 1176 | — |
| Reactant | 2-Bromo-4-chlorobenzoic acid | HCID 33126 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | 2-Bromo-4-chlorobenzonitrile | HCID 23498524 | — |
Reaction Steps
588 mg (2.5 mmol) of 2-bromo-4-chlorobenzoic acid and 300 mg of urea are dissolved in dichloromethane/methanol and concentrated onto 364 mg of alumina (neutral) on a rotary evaporator. The residue is microwaved at 150° C. for a total of 60 min. After cooling, the residue is stirred with ethyl acetate and water, filtered, and the aqueous phase is separated. The organic phase is washed with a sodium hydrogen carbonate solution, dried over sodium sulfate, concentrated on a rotary evaporator and then dried under high vacuum. The product (383 mg, 80% pure, 57% of theory.) is reacted further without additional purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977349B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-55b556c01c164b92bc29ab73a7a4ba3a |
| Source note | uspto-grants-2011_07 |