반응 #85044

반응 방정식

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

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   추출extracted three times with 300 ml of diethyl ether
3. 3
   건조The combined organic phases were dried over magnesium sulphate
4. 4
   여과filtered
5. 5
   기타the solvent was removed under reduced pressure
6. 6
   기타The crude product was used for the next step without further purification

실험 절차

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)

출처