Sulfuric Acid → 1-Hydroxy-3-(2,4,6-trichloro-phenyl)-propan-2-one

温度

28 °C

To an emulsion of dodecylsulfanyl-3-(2,4,6-trichloro-phenyl)-prop-2-en-1-ol (0.82 g; 1.9 mmol), prepared as described in example P61 in methanol (3 ml) was added dropwise 30% sulfuric acid (1.5 ml; 5.6 mmol). The temperature increased from 23° C. until 28° C. The mixture was heated at 60° C. for 5 h. Dioxane (2 ml) was added and reaction was stirred at 60° C. for 18 h. The biphasic mixture was transferred in a sealed microwave vial and heated at 80° C. for 10 min and at 100° C. for 10 min. The mixture obtained was poured in water and was extracted once with ethyl acetate. Organic layer was washed three times with water, dried over sodium sulfate and evaporated. The crude oil obtained was subject to flash chromatography (eluant: c-hexane/ethyl acetate 4:1). 80 mg (18% of theory) of 1-hydroxy-3-(2,4,6-trichloro-phenyl)-propan-2-one was obtained as a light yellow solid.

1. temperatureThe mixture was heated at 60° C. for 5 h
2. customreaction
3. temperatureheated at 80° C. for 10 min and at 100° C. for 10 min
4. customThe mixture obtained
5. extractionwas extracted once with ethyl acetate
6. washOrganic layer was washed three times with water
7. dry with materialdried over sodium sulfate
8. customevaporated
9. customThe crude oil obtained

ORDレコード

ord-5a7166a7720e4a3e9e2511e6181f034e

出典データセット

uspto-grants-2013_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08552049B2