反应详情

温度

25 °C

A mixture of N-ethyl-3-hydroxypiperidine (0.3 g, 2.3 mmol) and NaOH (94 mg, 2.3 mmol) in benzene (10 ml) was heated to reflux for 2 hr with stirring under nitrogen atmosphere and then cooled to 25° C. followed by the addition of compound 133 (0.3 g, 0.78 mmol) at same temperature. The mixture was heated to reflux for 12 hrs., concentrated under vacuum and diluted with water (10 ml). The solid precipitated was filtered off and washed with petroleum ether to afford the title compound as a off white solid (0.3 g, 81%). mp 62-64° C.; HPLC: HICHROM RPB (250×4.6 mm) 5 microns [solvent A=0.01 M KH2PO4 (pH 6.0); solvent B=CH3CN], Gradient elution program: T/% B=0/40, 5/40, 25/80, 35/80, 40/40, 45/40; 270 nm, Rt 26.83 min, 93.65% purity; MS (CI): m/z 447 (M+, 100).

1. temperaturewas heated
2. temperatureto reflux for 2 hr
3. temperatureThe mixture was heated
4. temperatureto reflux for 12 hrs
5. concentration, concentrated under vacuum
6. additiondiluted with water (10 ml)
7. customThe solid precipitated
8. filtrationwas filtered off
9. washwashed with petroleum ether