HRID1028956

反应详情

EQUATION

反应方程式

HRID 1028956 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

(2-(2-Amino-3-morpholinoquinolin-6-yl)phenyl)(tetrahydro-2H-pyran-4-yl)methanone (0.164 g, 0.393 mmol, see Example 11) was dissolved in MeOH (20 mL) and treated with sodium borohydride (0.021 mL, 0.589 mmol). After 10 min, the solution was heated to 40° C. for an additional 15 minutes, then evaporated to dryness under reduced pressure. The crude material was partitioned between water (20 mL), saturated sodium bicarbonate (20 mL), and ethyl acetate (40 mL). The organic layer was dried with magnesium sulfate and evaporated to dryness under reduced pressure and the crude material was purified by silica chromatography (10-100% hexane in ethyl acetate gradient. The product peak which eluted was concentrated to give (2-(2-amino-3-morpholinoquinolin-6-yl)phenyl)(tetrahydro-2H-pyran-4-yl)methanol. MS (ESI, pos. ion) m/z: 420 (M+1).

WORKUP

后处理

  1. customevaporated to dryness under reduced pressure
  2. customThe crude material was partitioned between water (20 mL), saturated sodium bicarbonate (20 mL), and ethyl acetate (40 mL)
  3. dry with materialThe organic layer was dried with magnesium sulfate
  4. customevaporated to dryness under reduced pressure
  5. customthe crude material was purified by silica chromatography (10-100% hexane in ethyl acetate gradient
  6. washThe product peak which eluted
  7. concentrationwas concentrated