HRID2216509

反应详情

EQUATION

反应方程式

HRID 2216509 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

To a suspension of LAH (52 mg, 1.36 mmol) in THF (6 ml) at 0° C., was added dropwise a solution of pyrazole ester 1.3 (500 mg, 1.24 mmol) in THF (3 ml). The mixture was stirred at 0° C. for 30 min, quenched with H2O, diluted with 1N HCl, and extracted with EtOAc (3×). The combined organic phase was washed with H2O, brine, and dried (Na2SO4). Filtration through a 1″ pad of SiO2, elution with ethyl acetate, and concentration of the filtrate afforded 448 mg (100%) alcohol 2.1. HRMS (ESI) calc'd for C23H27N2O2 363.1994; found 363.2083 (MH+).

WORKUP

后处理

  1. customquenched with H2O
  2. additiondiluted with 1N HCl
  3. extractionextracted with EtOAc (3×)
  4. washThe combined organic phase was washed with H2O, brine
  5. dry with materialdried (Na2SO4)
  6. filtrationFiltration through a 1″
  7. washpad of SiO2, elution with ethyl acetate, and concentration of the filtrate