HRID527876

反应详情

EQUATION

反应方程式

HRID 527876 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 7-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-4,7-diazaspiro[2.5]octane-4-carboxylic acid tert-butyl ester (intermediate 1) (0.5 g, mmol) dissolved in diethyl ether (20 ml) was added HCl in dioxane (ml, M) and the reaction mixture was stirred for 5 hours at room temperature. The precipitate was isolated by filtration, and washed with diethyl ether (2×5 ml). The precipitate was suspended in THF (50 ml) and stirred vigorously with K2CO3 (5 gram) for 3 hours. After filtration and evaporation of the solvent in vacuo, the product was obtained as an off-white compound.

WORKUP

后处理

  1. customThe precipitate was isolated by filtration
  2. washwashed with diethyl ether (2×5 ml)
  3. stirringstirred vigorously with K2CO3 (5 gram) for 3 hours
  4. filtrationAfter filtration and evaporation of the solvent in vacuo
  5. customthe product was obtained as an off-white compound