反応 #94828

反応方程式

21-chloro-20-methoxy-21-(phenylsulfinyl)pregna-4,9(11),17(20)-trien-3-one

21-Chloro-20-methoxy-21-(phenylsulfinyl)pregna-4,9(11),17(20)-trien-3-one

sodium hydroxide

water

methylene chloride

→

title compound

21-Chloro-17α-hydroxy-20-methoxypregna-4,9(11),20-trien-3-one

溶媒

THF

methanol

acetone

反応条件

後処理

1. 1
   その他is brought to 20°-25°
2. 2
   その他The layers are separated
3. 3
   抽出the aqueous layer is extracted with methylene chloride (2×5 ml)
4. 4
   洗浄washed with water (10 ml)
5. 5
   乾燥dried over sodium sulfate
6. 6
   濃縮concentrated under reduced pressure

実験手順

To a solution of 21-chloro-20-methoxy-21-(phenylsulfinyl)pregna-4,9(11),17(20)-trien-3-one (VI, Example 3, 100 mg) in THF (2 ml), methanol (0.45 ml) and acetone (0.3 ml) at 0° under nitrogen is added a solution of sodium hydroxide (5 N, 0.04 ml). The mixture is brought to 20°-25° and is allowed to stir for 24 hr. The mixture is poured into a mixture of water (25 ml) and methylene chloride (10 ml). The layers are separated and the aqueous layer is extracted with methylene chloride (2×5 ml). The organic extracts are combined and washed with water (10 ml), dried over sodium sulfate and concentrated under reduced pressure to give the title compound.

出典