HRID1798483

反应详情

EQUATION

反应方程式

HRID 1798483 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a solution of tert-Butyl (3R,4S)-3-({cyclopropyl[3-(4-methoxy-3,3-dimethyl-4-oxobutoxy)-5-(3-methoxypropyl)-benzyl]amino}carbonyl)-4-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]phenyl}-piperidine-1-carboxylate (1 eq.) from Example 21/Step 2 in ethanol was added 1 N aqueous NaOH (3 eq.). The reaction was heated to 100° C. for 10 min in a microwave reactor (Biotage). After cooling to rt, the reaction was concentrated in vacuo to removed the ethanol solvent. The resulting solution was acidified with 1 N HCl and extracted with ethyl acetate. The combined organic extracted were dried over anhydrous Na2SO4 and concentrated in vacuo. The crude product was used in the next step without further purification.

WORKUP

后处理

  1. temperatureAfter cooling to rt
  2. concentrationthe reaction was concentrated in vacuo
  3. customto removed the ethanol solvent
  4. extractionextracted with ethyl acetate
  5. extractionThe combined organic extracted
  6. dry with materialwere dried over anhydrous Na2SO4
  7. concentrationconcentrated in vacuo
  8. customThe crude product was used in the next step without further purification