反应详情

温度

60 °C

To a solution of tert-butyl nitrite (428 μL, 3.6 mmol) in N,N-dimethylformamide (5 mL) at 60° C. was dropwise added a solution of methyl 2-amino-5-phenylthiophene-3-carboxylate (11a) (420 mg, 1.8 mmol) in N,N-dimethylformamide (2.5 mL). The mixture was stirred at 60° C. for 1 hour, poured in water (15 mL) and extracted with ethyl acetate (2×20 mL). The organic layer was washed with brine (2×10 mL), dried over sodium sulfate and concentrated in vacuo. The residue was dissolved in toluene (5 mL) and concentrated in vacuo to provide the desired product (11b) (390 mg, 1.8 mmol, 99%) which was used without further purification.

1. extractionextracted with ethyl acetate (2×20 mL)
2. washThe organic layer was washed with brine (2×10 mL)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated in vacuo
5. dissolutionThe residue was dissolved in toluene (5 mL)
6. concentrationconcentrated in vacuo