反应详情

A solution of ammonia (1.2 ml) in tetrahydrofuran (100 ml) at -70° was contacted rapidly with a solution of 2-(1-chloroethyl)benzenesulfonyl chloride (4.32 g, 18.1 mmol) in tetrahydrofuran (50 ml). The stirred mixture was allowed to warm to 0° and volatiles were removed under reduced pressure. The residue was taken up in ethyl acetate and washed with a small volume of water and brine. The dried (MgSO4) solution was evaporated to give 4.7 g of off white solid which was recrystallized from chloroform to give 3.13 g, m.p. 121°-122°. 1H nmr δ(CD3)2COTMS 8.25-7.30 (m), 6.93 (brds), 6.25 (q, J=7 Hz), 3.17 (s), 1.98 (d, J=7 Hz).

1. customat -70°
2. temperatureto warm to 0°
3. customvolatiles were removed under reduced pressure
4. washwashed with a small volume of water and brine
5. dry with materialThe dried (MgSO4) solution
6. customwas evaporated
7. customto give 4.7 g of off white solid which
8. customwas recrystallized from chloroform
9. customto give 3.13 g, m.p. 121°-122°