反应详情

To a solution of isochroman-3,4-dione 4-oxime (98% pure, 3.5 g, 0.02 mol) in methanol (35 g) and dichlormethane (32 g) was added dropwise at 20-30° C. thionyl chloride (24.0 g, 0.2 mol). The resulting mixture was stirred at ambient temperature for 3 d. The reaction was monitored by HPLC. After completion of the reaction, the mixture was concentrated in vacuo and a crude residue was obtained (5.5 g). A part of this residue (5.1 g) was dissolved in MTBE and was washed with water. The mixture was concentrated and the resulting residue was purified by silica column chromatography by yield (2-chloromethyl-phenyl)-hydroxyimino-acetic acid methyl ester as a colorless solid (3.4

1. customAfter completion of the reaction
2. concentrationthe mixture was concentrated in vacuo
3. customa crude residue was obtained (5.5 g)
4. washwas washed with water
5. concentrationThe mixture was concentrated
6. customthe resulting residue was purified by silica column chromatography