HRID1401818

反应详情

EQUATION

反应方程式

HRID 1401818 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.2 g (6.22 mmol) of 5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalene-2-carboxylic acid hydrazide from step b were suspended in 15 ml of DMF together with 1.43 g (6.22 mmol) of 1-Boc-piperazine-4-carboxylic acid (preparation analogous to Bioorganic & Medicinal Chemistry Letters, 2001, vol. 11, #24 p. 3161-3164), 2.41 g (12.45 mmol) of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride and 867 mg (6.22 mmol) of 1-hydroxybenzotriazole hydrate. 1.40 ml (12.45 mmol) of 4-methylmorpholine were added to the reaction mixture, which was then stirred at room temperature overnight, stirred into 350 ml of water. The resultant precipitate was filtered off with suction, dissolved in DCM, dried, stripped off to dryness and purified by means of flash chromatography on silica gel.

WORKUP

后处理

  1. filtrationThe resultant precipitate was filtered off with suction
  2. dissolutiondissolved in DCM
  3. customdried
  4. custompurified by means of flash chromatography on silica gel