HRID589968

反应详情

EQUATION

反应方程式

HRID 589968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-(imidazole-1-sulfonyl)-piperidine (intermediate 13) (0.047 mmol) in dry CH2Cl2 (1 mL) was cooled to 0° C. and added trifluoro-methanesulfonic acid methyl ester (0.047 mmol). The reaction mixture was allowed to warm up freely to rt over a period of 4 h and then concentrated in vacuo. The residual oil was redissolved in dry CH3CN (1.5 mL), added a solution of 4-(4,7-diaza-spiro[2.5]oct-7-yl)-7H-pyrrolo[2,3-d]pyrimidine (intermediate 21) (0.047 mmol) in DMSO (1 mL) and then stirred at 50° C. for 3 h. The pure compound was obtained by standard preparative HPLC purification of the reaction mixture.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residual oil was redissolved in dry CH3CN (1.5 mL)
  3. customThe pure compound was obtained by standard preparative HPLC purification of the reaction mixture