反应详情

温度

0 °C

A solution of 7-nitro-1-trifluoroacteyl-1,2,3,4-tetrahydroquinoline (D4) (2 g, 7.3 mmol) in conc. sulfuric acid (10 ml) was cooled to 0° C. and treated with iodine (1.11 μg, 4.4 mmol) and potassium iodate (0.625 g, 2.9 mmol). The reaction was stirred at 0° C. for 3 h then room temperature for 2 h. The reaction mixture was slowly poured into water (150 ml) at 0° C. and extracted with DCM. This was washed with aq. sodium metabisulfite and water then dried over MgSO4 and concentrated in vacuo to give the crude product. Purification by column chromatography gave the title compound (420 mg). 1H NMR (250 MHz, CDCl3) δ (ppm): 8.59 (m, 2H), 3.86 (m, 2H), 2.90 (t, 2H), 2.17 (m, 2H).

1. waitroom temperature for 2 h
2. extractionextracted with DCM
3. washThis was washed with aq. sodium metabisulfite and water
4. dry with materialthen dried over MgSO4
5. concentrationconcentrated in vacuo
6. customto give the crude product
7. customPurification by column chromatography