HRID2043140

反应详情

EQUATION

反应方程式

HRID 2043140 的结构方程式

PROCEDURE

实验过程

Prepared using general procedure 13. To a stirring solution of sodium hydroxide (1.0M in H2O, 10 mL, 10 mmol), at 0° C., was added 4-(2-oxo-4-(2,2,2-trifluoroacetyl)piperazin-1-yl)-N-(pyrimidin-4-yl)benzenesulfonamide (0.45 g, 1.01 mmol) portionwise over 10 minutes. The mixture was stirred at ambient temperature for 30 minutes. The solution was cooled to 0° C. followed by the addition of 1.0 N HCl aqueous solution (10 mL, 10 mmol). The light yellow solution was azeotroped with MeOH (4×100 mL) at <30° C. The obtained solid was suspended in 50% MeOH in CH2Cl2 (200 mL) and stirred for 5 minutes. The mixture was filtered and the filtrate was evaporated to give the desired amine as light yellow solid (1.15 g, quantitative yield). LC/MS (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)), m/z: M+1 obs=334.1; tR=0.44 min.

WORKUP

后处理

  1. customPrepared
  2. temperatureThe solution was cooled to 0° C.
  3. customThe light yellow solution was azeotroped with MeOH (4×100 mL) at <30° C
  4. stirringstirred for 5 minutes
  5. filtrationThe mixture was filtered
  6. customthe filtrate was evaporated