反应详情

Methanesulphonyl chloride (58.3 g, 0.509 mole) was added in one portion to a stirred solution of 97% 4-chloro-3-nitroaniline (86 g, 0.485 mole) in pyridine (80 ml) and xylene (500 ml). The temperature rose to 50° and the mixture was allowed to stand for a further 2 hr before addition of a mixture of 10M-hydrochloric acid (100 ml) and water (100 ml). The brown solid which was collected and washed successively with xylene (50 ml) and water (3×50 ml). The damp material was crystallized from methanol (800 ml) to give a solid which was collected, washed with methanol (2×50 ml) and dried to give the product 95 g (78%) m.p. 163°.

1. customrose to 50°
2. customThe brown solid which was collected
3. washwashed successively with xylene (50 ml) and water (3×50 ml)
4. customThe damp material was crystallized from methanol (800 ml)
5. customto give a solid which
6. customwas collected
7. washwashed with methanol (2×50 ml)
8. customdried