反応 #3877

反応方程式

ethyl acetate

potassium carbonate

2-bromomethyl-5-ethoxy-1,3,4-thiadiazole

4-phenoxy phenol

→

compound

収率 74.2%

2-ethoxy-5-[(4-phenoxy)phenoxy]-methyl-1,3,4-thiadiazole

収率 74.2%

溶媒

acetone

反応条件

後処理

1. 1
   温度The resulting mixture was refluxed
2. 2
   温度heated for 2 hours
3. 3
   温度After cooling
4. 4
   洗浄by washing with water for two times
5. 5
   乾燥the resulting ethyl acetate layer was dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled over under reduced pressure
7. 7
   その他the residue was purified by chromatography on silica gel

実験手順

0.76 g of 4-phenoxy phenol was dissolved in 10 ml of acetone followed by adding 0.6 g of anhydrous potassium carbonate and 1.0 g of 2-bromomethyl-5-ethoxy-1,3,4-thiadiazole. The resulting mixture was refluxed with stirring and heated for 2 hours. After cooling, 100 ml of ethyl acetate was added followed by washing with water for two times, and the resulting ethyl acetate layer was dried over anhydrous magnesium sulfate. Ethyl acetate was distilled over under reduced pressure, and the residue was purified by chromatography on silica gel to obtain 1.0 g of the compound No. 1 described in Table 1.

出典