HRID1049282

反应详情

EQUATION

反应方程式

HRID 1049282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of diisopropyl 2-((1-(trifluoromethyl)cyclopropyl)methyl)malonate (1.53 g, 4.93 mmol) in MeOH (10 mL), dioxane (10 mL) and H2O (10 mL) was treated with NaOH (1.183 g, 29.6 mmol) and heated at 40° C. overnight. The mixture was cooled to RT, the organics removed under reduced pressure, the aqueous residue acidified with 3M HCl, extracted with DCM and the combined organics were dried over Na2SO4 and concentrated to dryness to afford 2-((1-(trifluoromethyl)cyclopropyl)methyl)malonic acid (1.13 g, 101%). 1H NMR (400 MHz, DMSO-d6): δ 12.91 (s, 2H), 3.36-3.34 (t, J=7.09 Hz, 1H), 2.08 (d, J=7.0 Hz, 2H), 0.88 (m, 2H), 0.77 (m, 2H).

WORKUP

后处理

  1. temperatureThe mixture was cooled to RT
  2. customthe organics removed under reduced pressure
  3. extractionextracted with DCM
  4. dry with materialthe combined organics were dried over Na2SO4
  5. concentrationconcentrated to dryness