HRID2355282

反应详情

EQUATION

反应方程式

HRID 2355282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 3-[(tert-butoxycarbonyl-methyl-amino)-methyl]-benzoic acid methyl ester (1.70 g, 6.1 mmol) in tetrahydrofuran (60 mL) at 0° C. Add a 1M solution of lithium aluminum hydride in tetrahydrofuran (8 mL, 8 mmol) dropwise and stir for 2 hrs. Quench the reaction with water (3 mL), 5N sodium hydroxide solution (3 mL) and more water (9 mL), filter and concentrate. Purify the residue by chromatography (silica gel) eluting with 40-60% ethyl acetate/hexanes to provide the title compound (1.42 g, 93%).

WORKUP

后处理

  1. customQuench
  2. customthe reaction with water (3 mL), 5N sodium hydroxide solution (3 mL) and more water (9 mL)
  3. filtrationfilter
  4. concentrationconcentrate
  5. customPurify the residue by chromatography (silica gel)
  6. washeluting with 40-60% ethyl acetate/hexanes