HRID1464022

反应详情

EQUATION

反应方程式

HRID 1464022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2,5-Bis(5-benzyloxycarbonyl-3-ethoxycarbonylmethyl-4-methylpyrrol-2-ylmethyl)-3,4-diethylpyrrole (11) (0.75 g, 1 mmol) was dissolved in 85 ml of dry THF and hydrogenated over 10% palladium-charcoal (41 mg) at 1 atm H2 until the reaction was deemed complete as judged by TLC. The catalyst was then separated by filtration, the solvent reduced in volume on the rotary evaporator, and the product precipitated by trituration with n-heptane. The white precipitate was collected by filtration and dried in vacuo to yield 0.56 g (98%) of 12 (m.p. 149° C. (dec.)), which was then used directly in the next step (the synthesis of 3, vide infra) without further purification.

WORKUP

后处理

  1. customThe catalyst was then separated by filtration
  2. customthe solvent reduced in volume on the rotary evaporator
  3. customthe product precipitated by trituration with n-heptane
  4. filtrationThe white precipitate was collected by filtration
  5. customdried in vacuo