反応 #1726662

反応方程式

1,3-diiodo-5,5-dimethylimidazolidine-2,4-dione

9-phenylanthracene

acetic acid

water

9-phenylanthracene

→

yellow solid

収率 117.3%

9-iodo-10-phenylanthracene

収率 117.3%

溶媒

chloroform

反応条件

後処理

1. 1
   洗浄This mixture was washed with water twice
2. 2
   抽出the aqueous layer was extracted with chloroform
3. 3
   洗浄washed with a saturated saline
4. 4
   乾燥the organic layer was dried with magnesium sulfate
5. 5
   ろ過filtered
6. 6
   濃縮the obtained filtrate was concentrated
7. 7
   その他to give a brown solid
8. 8
   洗浄This solid was washed with hexane

実験手順

Into a 500 mL Erlenmeyer flask was put 4.5 g (18 mmol) of 9-phenylanthracene. Then 200 mL of acetic acid was added to the flask, followed by heating to 70° C., and 9-phenylanthracene was dissolved therein. Into this solution, 5.2 g (13 mmol) of 1,3-diiodo-5,5-dimethylimidazolidine-2,4-dione (abbreviation: DIH) was added. This solution was stirred in air at 70° C. for 3 hours. After the stirring, about 100 mL of water and about 200 mL of chloroform were added to this solution. This mixture was washed with water twice, and the aqueous layer was extracted with chloroform. The extracted solution was combined with the organic layer and washed with a saturated saline, and then the organic layer was dried with magnesium sulfate. This mixture was gravity filtered, and the obtained filtrate was concentrated to give a brown solid. This solid was washed with hexane to give 5.8 g of a yellow solid, which was the object of the synthesis, in a yield of 86%.

出典