HRID1582942

反应详情

EQUATION

反应方程式

HRID 1582942 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 2-fluoro-4-(1-hydroxy-1-methyl-ethyl)-benzonitrile (1.95 g, 11.0 mmol) in tetrahydrofuran (30 mL) at 0° C. was added drop-wise a 1.0 M solution of lithium aluminium hydride in tetrahydrofuran (34 mL, 34.0 mmol). The reaction mixture was warmed to ambient temperature then refluxed for 30 minutes. The reaction mixture was cooled to 0° C., then quenched with methanol (20 mL) added drop-wise. The reaction mixture was then diluted with chloroform (700 mL) and washed with water (100 mL). The resulting suspension was filtered through Celite, after which the organic extract contained in the filtrate was separated, dried over magnesium sulfate (MgSO4), and concentrated to give 1.6 g 2-(4-aminomethyl-3-fluoro-phenyl)-propan-2-ol as an amber gum.

WORKUP

后处理

  1. temperaturethen refluxed for 30 minutes
  2. temperatureThe reaction mixture was cooled to 0° C.
  3. customquenched with methanol (20 mL)
  4. additionadded drop-wise
  5. additionThe reaction mixture was then diluted with chloroform (700 mL)
  6. washwashed with water (100 mL)
  7. filtrationThe resulting suspension was filtered through Celite
  8. extractionafter which the organic extract
  9. customwas separated
  10. dry with materialdried over magnesium sulfate (MgSO4)
  11. concentrationconcentrated