反応 #85044

反応方程式

ammonium chloride

tert-butyl 1,3-dithiane-2-carboxylate

1-iodo-2-methoxyethane

potassium tert-butoxide

→

tert-Butyl 2-(2-methoxyethyl)-1,3-dithiane-2-carboxylate

溶媒

dimethylformamide

反応条件

後処理

1. 1
   その他The resulting reaction mixture
2. 2
   抽出extracted three times with 300 ml of diethyl ether
3. 3
   乾燥The combined organic phases were dried over magnesium sulphate
4. 4
   ろ過filtered
5. 5
   その他the solvent was removed under reduced pressure
6. 6
   その他The crude product was used for the next step without further purification

実験手順

10.2 g (46.1 mmol) of tert-butyl 1,3-dithiane-2-carboxylate and 12.0 g (64.5 mmol) of 1-iodo-2-methoxyethane were initially charged in 127 ml of dimethylformamide, the mixture was cooled to 0° C. and 6.21 g (55.3 mmol) of potassium tert-butoxide were added. The resulting reaction mixture was stirred at 0° C. for 1 h and at RT for 16 h. The reaction mixture was added to 1.5 l of a 1:2 mixture of ice and saturated aqueous ammonium chloride solution and extracted three times with 300 ml of diethyl ether. The combined organic phases were dried over magnesium sulphate and filtered, and the solvent was removed under reduced pressure. The crude product was used for the next step without further purification. Yield: 11.1 g (87% of theory)

出典