HRID2093918

反应详情

EQUATION

反应方程式

HRID 2093918 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

4-({1-[4-(5-Cyclopropylmethoxy-1,3-benzodioxol-4-yl)-5H-pyrrolo[3,2-d]pyrimidin-7-yl]-methanoyl}-amino)-piperidine-1-carboxylic acid tert-butyl ester from example A86 (4.02 g; 7.5 mmol) is dissolved in warm (40-70° C.) 2-propanol (37.5 mL). After addition of 4M HCl in dioxane (7.5 mL) the stirred reaction mixture is heated to 80° C. for two hours. Tert-butylmethylether (150 mL) is added to the reaction mixture while still warm (40-70° C.). After cooling in an ice bath the precipitated product is collected, washed with tert-butylmethylether and dried in high vacuo at 50° C. to yield 3.35 g of the title compound as bright yellow solid.

WORKUP

后处理

  1. customthe stirred reaction mixture
  2. temperaturewhile still warm (40-70° C.)
  3. temperatureAfter cooling in an ice bath the precipitated product
  4. customis collected
  5. washwashed with tert-butylmethylether
  6. customdried in high vacuo at 50° C.