HRID2066468

反应详情

EQUATION

反应方程式

HRID 2066468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8-(2-chloro-4-morpholin-4-yl-thieno[3,2-d]pyrimidin-6-ylmethyl)-1,4-dioxa-8-aza-spiro[4.5]decane (0.97 g, 2.36 mmol) in 1,4-dioxane (16 mL) was slowly added concentrated HCl (24 mL) and the resulting solution was stirred at RT for 2 h. The reaction mixture was cooled to 0° C. and the pH was adjusted to 12 by careful addition of an aqueous solution of NaOH (50% w/v). EtOAc was added, the layers were separated and the aqueous layer was extracted further with EtOAc. The combined organic layers were dried (Na2SO4), then concentrated in vacuo to give the title compound as a yellow solid (0.9 g, 100%).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customthe layers were separated
  3. extractionthe aqueous layer was extracted further with EtOAc
  4. dry with materialThe combined organic layers were dried (Na2SO4)
  5. concentrationconcentrated in vacuo