Ammonium Chloride → Tert-butyl 2-(2-methoxyethyl)-1,3-dithiane-2-carboxylate

温度

0 °C

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)

1. customThe resulting reaction mixture
2. extractionextracted three times with 300 ml of diethyl ether
3. dry with materialThe combined organic phases were dried over magnesium sulphate
4. filtrationfiltered
5. customthe solvent was removed under reduced pressure
6. customThe crude product was used for the next step without further purification

ORDレコード

ord-23e59bb0f1e44d93a51a2c618ff37b6d

出典データセット

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09434690B2