HRID2230285

反应详情

EQUATION

反应方程式

HRID 2230285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the product from Example R (2(S)-[(azepane-1-carbonyl)-amino]-4-methyl-pentanoic acid benzyl ester) (38.5 g, 111 mmol) in 600 mL of THF was hydrogenated at 50 psi over 20% Pd/C (2.00 g) for 17 minutes. The reaction mixture was filtered through celite and concentrated to dryness. The residue was heated in 50 mL of hexane. The resulting suspension was cooled and the solid collected by filtration and washed with hexane. The solid was dried at room temperature under vacuum to give the title compound as a white solid (26.6 g, 93%), mp=88-89° C.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered through celite and
  2. concentrationconcentrated to dryness
  3. temperatureThe residue was heated in 50 mL of hexane
  4. temperatureThe resulting suspension was cooled
  5. filtrationthe solid collected by filtration
  6. washwashed with hexane
  7. customThe solid was dried at room temperature under vacuum