HRID1975422

反应详情

EQUATION

反应方程式

HRID 1975422 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of ethyl 4,4,4-trifluoro-2-methylbutyrate (7.7 g) in methanol (21 mL), tetrahydrofuran (21 mL) and water (8.4 mL) was treated with lithium hydroxide monohydrate (3.5 g). The mixture was stirred for 48 hours and the organic solvents evaporated. The resulting aqueous solution was diluted with water and acidified with 6N hydrochloric acid. The aqueous solution was exhaustively extracted with ethyl acetate. The combined organic extract was washed (water and brine), dried (MgSO4), filtered and evaporated to give 4,4,4-trifluoro-2-methylbutyric acid as a pale yellow liquid (6.5 g, 99%); partial NMR (300 MHz, CDCl3): 1.34 (d, 3H, CH3), 2.18 (m, 1H, H-C(3)), 2.67, (m, 1H, H-C(3)), 2.74 (m, 1H, H-C(2)), 10.6 (br, 1H, CO2H).

WORKUP

后处理

  1. customthe organic solvents evaporated
  2. additionThe resulting aqueous solution was diluted with water
  3. extractionThe aqueous solution was exhaustively extracted with ethyl acetate
  4. extractionThe combined organic extract
  5. washwas washed (water and brine)
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. customevaporated