HRID270229

反应详情

EQUATION

反应方程式

HRID 270229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Isopropylamine (4.0 mL) was dissolved in THF (20 mL). This solution was cooled to 0° C. and n-butyllithium (2.5 M, 20 mL) was added. The reaction was stirred for 90 min and then transferred to a solution of 2-fluoro-5-(trifluoromethyl)benzoic acid (4.2 g) in THF (40 mL) at-78° C. This mixture was stirred for 15 min and then quenched with aqueous NH4Cl. The mixture was extracted with EtOAc (3×), and the organic layer was dried, filtered, and concentrated in vacuo. Flash chromatography of the resulting residue provided 2-isopropylamino-5-(trifluoromethyl)benzoic acid (2.4 g). MS found: (M+H)+=248.2.

WORKUP

后处理

  1. custom78° C
  2. stirringThis mixture was stirred for 15 min
  3. customquenched with aqueous NH4Cl
  4. extractionThe mixture was extracted with EtOAc (3×)
  5. customthe organic layer was dried
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo