反应详情

Methanesulfonyl chloride (4.4 mL, 57 mmol) was added to a 0° C. dichloromethane (200 mL) solution containing 2-iodoaniline (5.0 g, 23 mmol) and triethylamine (9.6 mL, 69 mmol). The resulting mixture was stirred for 90 minutes, washed with HCl (0.5 M). The organics were separated then dried over sodium sulfate and concentrated in vacuo. The residue was then treated with potassium hydroxide (2.0 M in 1:1 methanol:water, 75 mL) for 30 min. This material was then diluted with dichloromethane and washed with HCl (1.0 N, 300 mL). The organics were separated then dried over sodium sulfate and concentrated to provide the title compound (5.15 g) as a tan solid.

1. washwashed with HCl (0.5 M)
2. customThe organics were separated
3. dry with materialthen dried over sodium sulfate
4. concentrationconcentrated in vacuo
5. additionThe residue was then treated with potassium hydroxide (2.0 M in 1:1 methanol:water, 75 mL) for 30 min
6. additionThis material was then diluted with dichloromethane
7. washwashed with HCl (1.0 N, 300 mL)
8. customThe organics were separated
9. dry with materialthen dried over sodium sulfate
10. concentrationconcentrated