反应详情

Dissolve 1,3-dichloro-2-methyl-5-nitrobenzene (0.50 g, 2.43 mmol) in DMF and treat with tin (II) chloride dihydrate (2.74 g, 12.1 mmol) in a single portion. Stir the reaction for 1 hour and dilute with ethyl acetate and filter through celite. Wash the filtrate four times with water and twice with brine, dry over MgSO4, filter and concentrate to a dark oil. Purify the residue by silica gel chromatography eluting with a gradient of 5% to 10% ethyl acetate in hexanes to give 342 mg (80%) of the titled product as white flakes.

1. customthe reaction for 1 hour
2. filtrationfilter through celite
3. washWash the filtrate four times with water
4. dry with materialtwice with brine, dry over MgSO4
5. filtrationfilter
6. concentrationconcentrate to a dark oil
7. customPurify the residue by silica gel chromatography
8. washeluting with a gradient of 5% to 10% ethyl acetate in hexanes