反应详情

2,6-Dichloro-benzaldehyde oxime (7.6 g, 40 mmol) is dissolved in 56 mL of DMF and N-chlorosuccinimide (5.9 g, 44.0 mmol) is added followed by a catalytic amount of HCl gas. The reaction mixture is stirred overnight. The reaction mixture is partitioned between ether and water. The layers are separated and the ether layer is washed with brine and is dried over sodium sulfate. The ether layer is filtered and the solvent is removed under reduced pressure to yield the crude product. The crude product is purified via chromatography using a gradient of 10% ethyl acetate in hexanes to 15% ethyl acetate in hexanes to yield the title compound. 1H-NMR (400 MHz, CDCl3) δ 8.76 (broad, 1H), 7.38-7.26 (m, 3H)

1. customThe reaction mixture is partitioned between ether and water
2. customThe layers are separated
3. washthe ether layer is washed with brine
4. dry with materialis dried over sodium sulfate
5. filtrationThe ether layer is filtered
6. customthe solvent is removed under reduced pressure
7. customto yield the crude product
8. customThe crude product is purified via chromatography