HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 13773036, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | HCID 13773037 | HCID 13773037 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 13773036 | HCID 13773036 | 86% |
Reaction Steps
A mixture of 4-(3-amino-2,6-difluorophenyl)-pyridine (6.5 g), acetic anhydride (4.9 g) and ethanol (200 ml) was heated at reflux. After 1 hour, a further 3.3 ml acetic anhydride was added and a third portion (1.5 ml) after another 3.5 hours. Reflux was continued for a total of 6 hours after which time the solution was cooled and evaporated and the residue was partitioned between aqueous sodium bicarbonate and chloroform. The organic layer was washed with water, dried and evaporated to give the solid product of m.p. 148°-150° C. (6.8 g, 86% yield). NMR (CDCl3, 60 MHz): 8.8 (m, 2H), 8.05 (m, 2H), 7.4 (m, 2H), 6.9 (m, 1H), 2.2 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04636506 |
| Source dataset | uspto-grants-1987_01 |
| ORD ID | ord-4f9bfcc1ba38465ea11cb9e619086b06 |
| Source note | uspto-grants-1987_01 |