HRID1728161

反应详情

EQUATION

反应方程式

HRID 1728161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Racemic (2′R,3R,4′S)-1′-(aminocarbonyl-methyl)-6-bromo-4′-(3-chlorophenyl)-2′-(1-methylene-propyl)-2,3-dihydro-2,6′-dioxo-spiro[indole-3,3′-piperidine]-1-methoxyethyl trimethylsilane (350 mg) was dissolved in a solution of trifluoroacetic acid (5 mL) and dichloromethane (5 mL). The reaction mixture was stirred at room temperature for 0.5 h. The reaction mixture was concentrated. The residue was redissolved in a mixture of methanol (3 ml) and DIPEA. The reaction tube was then placed into the cavity of a focused monomode microwave reactor and the contents of the flask were irradiated for 30 min at 120° C. The reaction mixture was concentrated and the residue was concentrated and the residue was purified by Prep-HPLC to obtain 70 mg product.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionThe residue was redissolved in a mixture of methanol (3 ml) and DIPEA
  3. customThe reaction tube was then placed into the cavity of a focused monomode microwave reactor
  4. customthe contents of the flask were irradiated for 30 min at 120° C
  5. concentrationThe reaction mixture was concentrated
  6. concentrationthe residue was concentrated
  7. customthe residue was purified by Prep-HPLC