HRID1842908

反应详情

EQUATION

反应方程式

HRID 1842908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 4-(1-(tert-butyldimethylsilyloxy)cyclopropyl)-N-(diphenylmethylene)-3-fluoroaniline (4.5 mg, 10.11 mmol, 1.0 eq) in THF (10 mL) was added 1N HCl (20 mL) and stirred vigorously for 1 h. The mixture was extracted with EtOAc (20 mL). The aqueous layer was basified with 1N aq. NaOH (30 mL) and extracted with EtOAc (50 mL). The combined organic layers were extracted with brine (20 mL) and dried over Na2SO4 and the solvent evaporated under vacuum; the resulting residue was purified by CC using EtOAc/PE (1:1) as eluent to get 1-(4-amino-2-fluorophenyl)cyclopropanol (0.7 g, 49%, yellow solid; TLC system: EtOAc/PE (1:1), Rf: 0.25).

WORKUP

后处理

  1. extractionThe mixture was extracted with EtOAc (20 mL)
  2. extractionextracted with EtOAc (50 mL)
  3. extractionThe combined organic layers were extracted with brine (20 mL)
  4. dry with materialdried over Na2SO4
  5. customthe solvent evaporated under vacuum
  6. customthe resulting residue was purified by CC