Sulfuric Acid → 4,4,4-Trifluoro-3-methylbut-2-en-1-ol

To a solution of 4.5 g of ethyl 4,4,4-trifluoro-3-methyl-2-butenoate in 50 ml of tetrahydrofuran was added dropwise 48 ml of diisobutylaluminum hydride (1.02M solution in hexane) under ice-cooling. The reaction mixture was stirred at the same temperature for 2 hours. To the reaction mixture was added diluted sulfuric acid and then extracted with t-butyl methyl ether. The organic layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure to obtain crude 4,4,4-trifluoro-3-methyl-2-buten-1-ol.

1. temperaturecooling
2. extractionextracted with t-butyl methyl ether
3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure

ORDレコード

ord-5cd26017bd1b418980424a307e553aab

出典データセット

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08247595B2