HRID1486898

反应详情

EQUATION

反应方程式

HRID 1486898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of tert-butyl 3-(4-(4-(benzyloxy)-2-(5,5-bis(2-tert-butoxy-2-oxoethyl)-4,5-dihydro-1,2-oxazol-3-yl)phenyl)-3,6-dihydropyridin-1(2H)-yl)propanoate (245 mg), 10% Pd/C (containing about 55% water, 25 mg), and THF (3 mL) was stirred at room temperature for 3 hours under a hydrogen atmosphere. The catalyst was filtered off, and then, the filtrate was concentrated under reduced pressure. The obtained residue was mixed with 10% Pd/C (containing about 55% water, 50 mg) and THF (3 mL). The obtained mixture was stirred at room temperature for 3 hours under a hydrogen atmosphere. The catalyst was filtered off, and then, the filtrate was concentrated under reduced pressure. The obtained residue was mixed with 10% Pd/C (containing about 55% water, 75 mg) and THF (3 mL). The obtained mixture was stirred overnight at room temperature under a hydrogen atmosphere. The catalyst was filtered off, and then, the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (60.7 mg).

WORKUP

后处理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionThe obtained residue was mixed with 10% Pd/C (containing about 55% water, 50 mg) and THF (3 mL)
  4. stirringThe obtained mixture was stirred at room temperature for 3 hours under a hydrogen atmosphere
  5. filtrationThe catalyst was filtered off
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. additionThe obtained residue was mixed with 10% Pd/C (containing about 55% water, 75 mg) and THF (3 mL)
  8. stirringThe obtained mixture was stirred overnight at room temperature under a hydrogen atmosphere
  9. filtrationThe catalyst was filtered off
  10. concentrationthe filtrate was concentrated under reduced pressure
  11. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)