Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Dichloromaleic anhydride | HCID 70728 | — |
| Reactant | HCID 13783234 | HCID 13783234 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 14837272 | HCID 14837272 | — |
Reaction Steps
The hydrochloride thus obtained (1.0 g) was dissolved in 25 ml of tetrahydrofuran and allowed to react with 1.2 ml of triethylamine at room temperature for 30 minutes, the precipitated crystals were separated by filtration, and the filtrate concentrated under a reduced pressure to give a colorless oily product. This oily product and 700 mg of dichloromaleic anhydride were dissolved in 6 ml of acetic acid and refluxed for 3 hours, and after completion of the reaction, the reaction mixture was concentrated under a reduced pressure, the residue was dissolved in ethyl acetate, washed with water, and dried over magnesium sulfate, followed by evaporation of the solvent. The residue obtained was purified by silica gel chromatography (eluant: n-hexane-ethyl acetate=9/1) to give 1.41 g of the desired compound as a colorless oily product (yield: 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05039696 |
|---|
| Source dataset | uspto-grants-1991_08 |
|---|
| ORD ID | ord-6f827aa7dc5b4828ad15a50ed6edc295 |
|---|
| Source note | uspto-grants-1991_08 |
|---|