Ethanol → [2-Chloro-5-hydroxyphenyl]ethyl acetate

温度

80 °C

To a mixture of [2-chloro-5-(methoxymethoxy)phenyl]acetonitrile (2.60 g; 12.3 mmol), sodium hydroxide (2.46 g; 61.5 mmol), water (10.4 ml) and ethanol (33.8 ml) was stirred at 80° C. for 3 hours. After cooling, the solvent was evaporated under reduced pressure. To the residue was added water and 2N-aqueous hydrochloric acid to become acid and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulphate, and evaporated under reduced pressure. To the residue, were added concentrated hydrochloric acid (0.65 ml) and ethanol (15 ml). The mixture was stirred at 80° C. for 8 hours. After cooling, the reaction solution was condensed under reduced pressure. The residue was purified by column chromatograph on silica gel (hexane:ethyl acetate=2:1) to give [2-chloro-5-hydroxyphenyl]ethyl acetate as colorless oil (0.69 g; 26%).

1. temperatureAfter cooling
2. customthe solvent was evaporated under reduced pressure
3. additionTo the residue was added water and 2N-aqueous hydrochloric acid
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with brine
6. dry with materialdried over anhydrous sodium sulphate
7. customevaporated under reduced pressure
8. additionTo the residue, were added concentrated hydrochloric acid (0.65 ml) and ethanol (15 ml)
9. stirringThe mixture was stirred at 80° C. for 8 hours
10. temperatureAfter cooling
11. customcondensed under reduced pressure
12. customThe residue was purified by column chromatograph on silica gel (hexane:ethyl acetate=2:1)

ORDレコード

ord-0b4079b6f32f4ba49d0884a4bea5f60b

出典データセット

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08097610B2