HRID1678443

反应详情

EQUATION

反应方程式

HRID 1678443 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of ethyl 1-[4-chloro-6-(methylamino)-1,3,5-triazin-2-yl]-4-piperidinecarboxylate (983 mg, 3.28 mmol, 1.00 equiv) in tetrahydrofuran (21 ml) at 0° C., a premixed solution of lithium hydroxide monohydrate (275 mg, 6.56 mmol, 2.00 equiv) and water (7 ml) was added dropwise. Methanol (7 ml) was added. The reaction was allowed to warm to room temperature over 1 h and stirring was continued for 3 h. The solvent was removed under reduced pressure, yielding a colorless oil. Ethyl acetate was added to the oil, and the desired product precipitated as a white solid. The solid was filtered and dried under reduced pressure to provide 885 mg (99%) of the title compound. MS (ES+): m/e 272.0 [M+H]+.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customyielding a colorless oil
  3. customthe desired product precipitated as a white solid
  4. filtrationThe solid was filtered
  5. customdried under reduced pressure