HRID844868

反应详情

EQUATION

反应方程式

HRID 844868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of 3-methyl-6-(trifluoromethyl)uracil (20.6 mmol, 4.0 g) and powdered potassium carbonate (41.2 mmol, 5.7 g) in DME (30 mL) was added methyl iodide (82.4 mmol, 5.13 mL). Then, the reaction mixture was refluxed for 4 h at which time the TLC analysis of the reaction mixture indicated the absence of starting material. The reaction mixture was cooled to room temperature and was diluted with water (50 mL). Then, the DME was removed under reduced pressure to afford a white suspension. The solids were collected by filtration and washed with water. After air drying, 3.55 g (83% yield) of 1,3-dimethyl-6-(trifluoromethyl)uracil was obtained as a white solid: mp 85-87° C. EI-HRMS m/e calcd for C7H7F3N2O2 (M+) 208.0459, found 208.0460.

WORKUP

后处理

  1. temperatureThen, the reaction mixture was refluxed for 4 h at which time the TLC analysis of the reaction mixture
  2. customThen, the DME was removed under reduced pressure
  3. customto afford a white suspension
  4. filtrationThe solids were collected by filtration
  5. washwashed with water
  6. customAfter air drying