反应详情

To a suspension of anhydrous N,N-dimethylformaide (30 ml) containing sodium hydride (0.35 g, 55% (w/w)) was added 4-amino-3,5-dimethylphenol (1.10 g) and the mixture was stirred at room temperature for 15 minutes. To the mixture was added in limited amounts t-butyl N-(5-chloro-2-nitrophenyl)-N-methylcarbamate (2.29 g) and the mixture was stirred at 120° C. for 1 hour. The reaction mixture was concentrated and partitioned between ethyl acetate and water. The extract was dried over anhydrous sodium sulfate and concentrated. The residue was chromatographed on a silica gel column using ethyl acetate:n-hexane=1:3 as the eluant to afford the desired compound (2.27 g, Rf=0.24: thin layer chromatography on a silica gel plate using ethyl acetate:n-hexane=1:3 as the eluant).

1. additionTo a suspension of anhydrous N,N-dimethylformaide (30 ml)
2. stirringthe mixture was stirred at 120° C. for 1 hour
3. concentrationThe reaction mixture was concentrated
4. custompartitioned between ethyl acetate and water
5. dry with materialThe extract was dried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe residue was chromatographed on a silica gel column