HRID2263720

反应详情

EQUATION

反应方程式

HRID 2263720 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Prepared in the microwave oven (EmrysOptimizer®). 4-Methyl-5-(4-methyl-piperazine-1-sulfonyl)-thiazol-2-ylamine (0.04 g; 0.141 mmol), CDI (0.023 g; 0.141 mmol) and DMAP were mixed dichloroethane (1.5 ml) in a microwave vessel (2.5 ml). The reaction mixture was heated 600 sec at 120° C., dicyclohexylamine (0.025 g; 0.141 mmol) dissolved in dichloroethane (0.2 ml) was added through the septum and the reaction mixture was heated for additional 600 sec. at 120° C. To the reaction mixture was added water and DCM (25 ml). The water phase was extracted with DCM (3×25 ml), dried with MgSO4 filtered and evaporated in vacuo to afford the title compound, (84 mg) as a yellow oil. Purification by prep. HPLC gave 3 mg (Yield: 4%)

WORKUP

后处理

  1. customPrepared in the microwave oven (EmrysOptimizer®)
  2. additionwas added through the septum
  3. temperaturethe reaction mixture was heated for additional 600 sec
  4. customat 120° C
  5. extractionThe water phase was extracted with DCM (3×25 ml)
  6. dry with materialdried with MgSO4
  7. filtrationfiltered
  8. customevaporated in vacuo