HRID1292044

反应详情

EQUATION

反应方程式

HRID 1292044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of LAH (0.64 g, 17.0 mmol) in THF (30 mL) at -78° C. was added dropwise methyl 4-trifluoromethylnicotinate (1.74 g, 8.48 mmol) in THF (20 mL). The mixture was stirred for 1 h then carefully quenched with aqueous NaHCO3 (80 mL) and extracted with CH2Cl2 (3×100 mL). The combined organic extracts were dried (Na2SO4) and concentrated in vacuo to give 3-hydroxymethyl-4-trifluoromethylpyridine as an oil (TLC: Rf = 0.35 (1:1 hexane:EtOAc)).

WORKUP

后处理

  1. customthen carefully quenched with aqueous NaHCO3 (80 mL)
  2. extractionextracted with CH2Cl2 (3×100 mL)
  3. dry with materialThe combined organic extracts were dried (Na2SO4)
  4. concentrationconcentrated in vacuo