반응 #1068535

반응 방정식

2,6-dibromo-6-bromomethylandrost-4-ene-3,17-dione

sodium iodide

→

crude title compound

수율 98.8%

2-Bromo-6-methylenandrost-4-ene-3,17-dione

수율 98.8%

용매

acetone

반응 조건

후처리

1. 1
   기타A 250 ml 3-necked round bottomed flask fitted with a condenser
2. 2
   온도The resulting suspension in refluxed for 15 min
3. 3
   여과filtered
4. 4
   기타evaporated in vacuo
5. 5
   세척washed twice with a saturated sodium thiosulfate aqueous solution, twice with water
6. 6
   건조dried over anhydrous calcium chloride
7. 7
   기타Evaporation of the solvent in vacuo

실험 절차

A 250 ml 3-necked round bottomed flask fitted with a condenser, a thermometer and a magnetic stirrer is charged with 2.68 g of 2,6-dibromo-6-bromomethylandrost-4-ene-3,17-dione, 100 ml of acetone and 5.99 g of sodium iodide. The resulting suspension in refluxed for 15 min, cooled to room temperature, filtered and evaporated in vacuo. The residue is taken up with 50 ml of chloroform, washed twice with a saturated sodium thiosulfate aqueous solution, twice with water and dried over anhydrous calcium chloride. Evaporation of the solvent in vacuo yields 1.86 g of the crude title compound which is directly used for the next step.

출처