11alpha-Hydroxyprogesterone → HCID 18595303、化合物

関与物質

反応手順

A mixture of 11α-hydroxy progesterone (6 g., 0.018 mole), anhydrous lithium chloride (6 g., 0.14 mole), N-(2-Chloro-1,1,2-trifluoroethyl)diethylamine (6 ml., 0.036 mole) and dry tetrahydrofuran (120 ml.) was stirred at -20° for 5 hr. and then room temperature for 16 hr. The reaction mixture was partitioned between methylene chloride and water. Evaporation of the organic layer and chromatography of the residue on magnesium silicate afforded, after recrystallisation from acetone/petroleum ether (b.p. 60°-80°), 11β-chloropregn-4 -ene-3,20-dione (0.26 g., 4%), m.p. 185°-188° [α]D + 252° (c 1.0 CHCl3), λmax. (EtOH) 238 nm. (ε 17,150).

情報源と証拠