HRID726898

反应详情

EQUATION

反应方程式

HRID 726898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dissolve 6-hydroxynorleucine (14.7 g, 0.1 mol) in 1N sodium hydroxide (200 mL, 0.2 mol). Add a solution of CuSO4.5H2O (12.5 g, 0.05 mol) in water (50 mL). Stir the mixture until solution is complete. Treat with benzyl bromide (17.1 g, 0.1 mol) and stir at room temperature until reaction is complete. Suction filter, wash the residue with 1:3.5 methanol-water and dry at 60° C. to give the copper complex. Suspend the copper complex in water, treat with excess hydrogen sulfide, heat to boiling, then cool to room temperature. Mix with 1N sodium hydroxide and filter. Stir the filtrate with a slight excess of 1N hydrochloric acid and filter. Wash the residue with water and dry to give O-benzyl-6-hydroxynorleucine.

WORKUP

后处理

  1. stirringstir at room temperature until reaction
  2. filtrationSuction filter
  3. washwash the residue with 1:3.5 methanol-water
  4. customdry at 60° C.
  5. customto give the copper complex
  6. temperatureheat
  7. filtrationfilter
  8. stirringStir the filtrate with a slight excess of 1N hydrochloric acid
  9. filtrationfilter
  10. washWash the residue with water
  11. customdry