HRID520819

反应详情

EQUATION

反应方程式

HRID 520819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
250 °C

PROCEDURE

实验过程

To a suspension of 2-amino terephthalic acid (12 g, 6.6 mmols) in diphenyl ether (120 mL), cyclohexanone (25 mL) was added and the reaction mixture was heated to 250° C. for 10 min. Reaction completion was monitored by LC/MS (75% starting material and 25% Product formation was observed). Cyclohexanone (25 mL) was added and the reaction mixture was heated to 250° C. for another 10 min. (LC/MS showed 50% product formation). The above process was repeated till LC/MS showed complete product formation (Starting material <2%). The reaction mixture was cooled to 25° C., product was filtered, washed with hexane (100 mL) and dried under vacuum to get 15.8 g of (Via) (98%) as a yellow solid.

WORKUP

后处理

  1. additionwas added
  2. customReaction completion
  3. temperatureThe reaction mixture was cooled to 25° C.
  4. filtrationproduct was filtered
  5. washwashed with hexane (100 mL)
  6. customdried under vacuum
  7. customto get 15.8 g of (Via) (98%) as a yellow solid