HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 72321882, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl 2-methylacetoacetate | HCID 701 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium Nitrate | HCID 24268 | — |
| Reactant | 4-Fluoro-2-nitroaniline | HCID 67769 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 72321882 | HCID 72321882 | 46% |
Reaction Steps
4-Fluoro-2-nitroaniline (10 g, 64 mmol) was dissolved in 6N hydrochloric acid (64 ml, 0.27 mol), sodium nitrate (4.4 g, 64 mmol) dissolved in water (50 ml) was slowly added in drops at 0° C., and the mixture was stirred for 30 min at 0° C.˜room temperature. At the same time, ethyl 2-methylacetoacetate (9.2 ml, 64 mmol) and sodium hydroxide (19 g, 0.34 mol) were dissolved in 80% ethanol aqueous solution (95 ml) and stirred for 10 min at 0° C. Thus prepared two solutions were mixed and stirred for 8 h at 0° C.˜room temperature. To the reaction mixture was added water. The solid not dissolved was collected, washed with water and dried to give the title compound (7.9 g, Yield 46%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08349885B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-e34920ce22224371abf39c87a5a2dbeb |
| Source note | uspto-grants-2013_01 |