HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → 1,3-Difluoro-5-(2-nitroethenyl)benzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | 1-(3,5-Difluorophenyl)-2-nitroethanol | HCID 68562553 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1,3-Difluoro-5-(2-nitroethenyl)benzene | HCID 67348789 | 73.2% |
Reaction Steps
Add acetic anhydride (160 mL) to a solution of 1-(3,5-difluorophenyl)-2-nitroethanol (330 g) and 4-dimethylaminopyridine (18 g) in dichloromethane (1000 mL), over 30 minutes and stir the reaction mixture overnight. Dilute with dichloromethane (600 mL) and wash with 2% aqueous hydrochloric acid, saturated aqueous sodium chloride, saturated aqueous sodium bicarbonate, dry (magnesium sulfate) and concentrate. Wash the crude with hexanes to give the desired compound (220 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07745438B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-1080cca5ae27486f9ef3c8ea4c9fcc42 |
| Source note | uspto-grants-2010_06 |