HRID733680

反应详情

EQUATION

反应方程式

HRID 733680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

A mixture of 7-chloro-1H-pyrrolo[2,3-c]pyridine-4-carboxylic acid (tetrahydro-pyran-4-ylmethyl)-amide (20 mg), 3-chloroaniline (15 ul), and methanesulfonic acid (9 ul) in 1,4-dioxane (0.5 ml) was heated under microwave conditions at 180° C. for 30 minutes. The solid mass obtained was dissolved in methanol, transferred to a round bottom flask and evaporated. The residue was partitioned between ethyl acetate and 5% sodium hydrogen carbonate solution whereby the title compound remained as a solid at the interface. The solid was filtered off, and washed with 5% sodium hydrogen carbonate solution, water and diethyl ether, then sucked dry and dried at 60° C. under vacuum to afford the title compound (17 mg).

WORKUP

后处理

  1. customThe solid mass obtained
  2. customtransferred to a round bottom flask
  3. customevaporated
  4. customThe residue was partitioned between ethyl acetate and 5% sodium hydrogen carbonate solution whereby the title compound
  5. filtrationThe solid was filtered off
  6. washwashed with 5% sodium hydrogen carbonate solution, water and diethyl ether
  7. customsucked dry
  8. customdried at 60° C. under vacuum