反应详情

2-Mesitylenesulfonyl chloride (24.78 g, 0.113 mol) in pyridine (60 ml) was added all at once to 4-piperidineethanol (5.58 g, 43.2 mmol) in pyridine (25 ml) at -16° C.; the temperature rose to -11° C. The flask was stored in the refrigerator at 5.5° C. for 44 hours under argon. The reaction mixture was poured into ice (1 kg) and after 3 hours, 16.00 g (75%) of (2) as a yellow solid was filtered off: mp 93.5°-94° C.; NMR (CDCl3 /TMS) δ 1.4-2.1 (m, 7H), 2.27 (s, 6H), 2.44-2.96 (m+s, 14H), 3.37-3.69 (m, 2H), 3.97 (t, 2H, J=5), 6.90 and 6.93 (2s, 4H). Anal. calcd. for C25H35NO5S5 : C-60.82, H-7.15, N-2.84. Found: C-60.90, H-7.13, N2.85.

1. customrose to -11° C
2. filtration16.00 g (75%) of (2) as a yellow solid was filtered off