HRID40211

反应详情

EQUATION

反应方程式

HRID 40211 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 1-(6-chloropyridazin-3-yl)hydrazine (1.67 g, 12 mmol), 2-(quinolin-6-yl)acetic acid (1.65 g, 8.8 mmol), and HCl (2000 μl, 24 mmol) was heated in an oil bath at 110° C. for 20 min before it was heated in a microwave (Personal Chemistry) at 180° C.& 15 min. The mixture was quenched with a solution of NaOH (1.2 g, 5 mL) slowly until the suspension is neutral in pH. The mixture was filtered and washed with H2O (2×5 mL). A brown solid was obtained (2.2 g). The solid was treated with aqueous Na2CO3 (3 g, 20 mL, pH ˜11) and heated at 50° C. for 30 min. The blue mixture was cooled to room temperature, and filtered. The black solid was washed with H2O and lyophilized to give the product.

WORKUP

后处理

  1. temperaturewas heated in a microwave (Personal Chemistry) at 180° C.
  2. custom15 min
  3. customThe mixture was quenched with a solution of NaOH (1.2 g, 5 mL) slowly until the suspension
  4. filtrationThe mixture was filtered
  5. washwashed with H2O (2×5 mL)
  6. customA brown solid was obtained (2.2 g)
  7. temperatureheated at 50° C. for 30 min
  8. temperatureThe blue mixture was cooled to room temperature
  9. filtrationfiltered
  10. washThe black solid was washed with H2O
  11. customto give the product