反应详情

温度

105 °C

A suspension of 2α,3α-epoxy-16β-(1-pyrrolidinyl)-5α-androstan-17β-ol (1.80 Kg, 5.006 mol) in a mixture of morpholine (11.44 L) and purified water (1.144 L) was prepared at 20-24° C. and under N2 atmosphere. To the suspension was added p-toluenesulphonic acid (1.24 Kg, 6.508 mol) at 20-24° C. and under N2 atmosphere. The suspension was stirred in the darkness and heated to reflux (100-110° C.) for 40 h. After 40 h the reaction mixture was cooled to 20-24° C., and poured into a second vessel maintained at about 4° C. containing a 2% s solution of sodium carbonate (128 L), while stirred vigorously. The resulting suspension was stirred for 1 hour at about 4° C. The obtained solid was filtered off under vacuum, washed with cold purified water (100 L), and dried in a vacuum oven at about 40° C. for at least 48 hours, to give 2.07 Kg (4.49 mol) of a white solid. (89.7% molar yield and purity of 94.12% area by HPLC) m.p. 225° C.; [α]D20+82.00 (c=1.02 in CHCl3). The product could be used in the next stage without further purification.

1. custompurified water (1.144 L)
2. customwas prepared at 20-24° C. and under N2 atmosphere
3. temperatureheated
4. temperatureAfter 40 h the reaction mixture was cooled to 20-24° C.
5. additionpoured into a second vessel
6. temperaturemaintained at about 4° C.
7. additioncontaining a 2%
8. stirringwhile stirred vigorously
9. stirringThe resulting suspension was stirred for 1 hour at about 4° C
10. filtrationThe obtained solid was filtered off under vacuum
11. washwashed
12. customwith cold purified water (100 L)
13. customdried in a vacuum oven at about 40° C. for at least 48 hours