HRID526766

反应详情

EQUATION

反应方程式

HRID 526766 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-iodo-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carboxylic acid (34 g, 105 mmol) in BH3-THF (340 mL, 340 mmol, 1M in THF) was stirred at rt overnight. Solvent was evaporated under vacuum and the residue dissolved in DCM (340 mL), washed with water (340 mL×3), dried and concentrated. The residue was purified by SGC using Hex: EA (0%-70%) as eluent to afford (3-iodo-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl)methanol (27 g, yield: 83%). LCMS (method C): RT=1.74 min, m/z=309.1 [M+H]+.

WORKUP

后处理

  1. customSolvent was evaporated under vacuum
  2. dissolutionthe residue dissolved in DCM (340 mL)
  3. washwashed with water (340 mL×3)
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by SGC