反応 #1992192

反応方程式

6α-azido-1,2β-methylenandrost-4-ene-3,17-dione

1,3-propanedithiol

triethylamine

→

6α-amino-1,2β-methylenandrost-4-ene-3,17-dione

収率 64.0%

溶媒

methanol

反応条件

後処理

1. 1
   その他Then the reaction mixture is evaporated in vacuo to dryness
2. 2
   洗浄the etheral solution washed with water
3. 3
   その他dried
4. 4
   その他evaporated in vacuo

実験手順

A mixture of 6α-azido-1,2β-methylenandrost-4-ene-3,17-dione (1695 mg, 5 mmol), 1,3-propanedithiol (0.25 ml, 2.5 mmol), triethylamine (0.35 ml, 2.5 mmol) and methanol (2.5 ml) is stirred for 6 hours at room temperature. Then the reaction mixture is evaporated in vacuo to dryness. The residue is taken up in ether, the etheral solution washed with water, dried and evaporated in vacuo. Column chromatography of the residue over silica gel affords the pure 6α-amino-1,2β-methylenandrost-4-ene-3,17-dione (1000 mg, 64%).

出典