HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4,5,6-Tetrahydrophthalic anhydride → HCID 14423596, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4,5,6-Tetrahydrophthalic anhydride | HCID 12475 | — |
| Reactant | HCID 14423583 | HCID 14423583 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 14423596 | HCID 14423596 | 80.5% |
Reaction Steps
A mixture of 6-amino-7-fluoro-4-(pyridin-2-ylmethyl)-2H-1,4-benzoxazin-3(4H)-one (2 g), 3,4,5,6-tetrahydrophthalic anhydride (1.2 g) and acetic acid (50 ml) was heated under reflux for 1 hour. The acetic acid was distilled off under a reduced pressure, and the residue was dissolved in toluene (100 ml), washed in a saturated aqueous solution of sodium bicarbonate and then in water, and dried over anhydrous sodium sulfate. The toluene was distilled off under a reduced pressure, and the resultant residue was recrystallized from ethanol, whereby the aimed product, namely, 7-fluoro-4-(pyridin-2-ylmethyl)-6-(4,5,6,7-tetrahydro-2H-isoindole-1,3-dion-2-yl)-2H-1,4-benzoxazin-3(4H)-one (2.4 g) was obtained. m.p. 188°-190° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04902335 |
| Source dataset | uspto-grants-1990_02 |
| ORD ID | ord-32bdb40ad5084a049b34f8fa13613850 |
| Source note | uspto-grants-1990_02 |