HRID1663415

反应详情

EQUATION

反应方程式

HRID 1663415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Sodium 2-propanethiolate (58.5 mg, 0.596 mmol) was added to a solution of methyl 2-methyl-2-(3-(4-(morpholine-4-carbonyl)phenyl)-10H-chromeno[3,2-c]pyridin-10-yl)propanoate (140.9 mg, 0.298 mmol) in DMF (5 mL) and the mixture was heated to 50° C. After 1 h at 50° C., additional sodium 2-propanethiolate (58.5 mg) was added. The mixture was stirred at 50° C. overnight. Another portion of sodium 2-propanethiolate (200 mg) was added. After another hour at 50° C., the mixture was quenched with saturated NH4Cl (20 mL) and extracted with EtOAc (4×20 mL). The combined extracts were washed with brine (5 mL), dried (MgSO4) and concentrated to give 2-methyl-2-(3-(4-(morpholine-4-carbonyl)phenyl)-10H-chromeno[3,2-c]pyridin-10-yl)propanoic acid as a solid (145.5 mg). MS (ES+) m/z: 459 (M+H); HPLC retention time: 3.51 min (Analytical HPLC Method D).

WORKUP

后处理

  1. waitAfter another hour at 50° C.
  2. customthe mixture was quenched with saturated NH4Cl (20 mL)
  3. extractionextracted with EtOAc (4×20 mL)
  4. washThe combined extracts were washed with brine (5 mL)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated