HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 13770519, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 2,4-Difluoroaniline | HCID 9709 | — |
| Reactant | HCID 13770533 | HCID 13770533 | — |
| Solvent | Benzene | HCID 241 | — |
| Product | HCID 13770519 | HCID 13770519 | 80% |
Reaction Steps
A mixture of 1.0 g. (3.1 mmoles) of ethyl 1-ethyl-5-(2-methyl-4,5-dihydro-1,3-dioxol-2-yl)oxindole-3-carboxylate and 809 mg. (6.3 mmoles) of 2,4-difluoroaniline in 40 ml of benzene was heated to reflux through a soxhlet filled with 4A sieves for 45 minutes. The reaction mixture was cooled and poured into a mixture of 400 ml. 2N hydrochloric acid and 100 ml. of methylene chloride. The organic layer was separated, dried over magnesium sulfate and concentrated to give 1.24 g. of a solid residue. Recrystallization from diisopropyl ether - methylene chloride gave 1.0 g. of product (80% yield), m.p. 166°-170° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04686224 |
| Source dataset | uspto-grants-1987_08 |
| ORD ID | ord-fbaca76123ad49008aae318ff22f3088 |
| Source note | uspto-grants-1987_08 |