HRID1608923

反应详情

EQUATION

反应方程式

HRID 1608923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 32.9 mL (0.033 mole) of boron tribromide (1M in methylene chloride) in 50 mL of methylene chloride was stirred, and a solution of 3.5 grams (0.011 mole) of 3-(2-fluoro-4-methoxyphenyl)-1-methyl-6-trifluoromethyluracil in 50 mL of methylene chloride was added dropwise. Upon completion of addition, the reaction mixture was stirred at ambient temperature for about 18 hours. After this time the reaction mixture was poured into water. The organic layer was separated and the aqueous layer was extracted with methylene chloride. The methylene chloride extract and the organic layer were combined and washed with water. The organic layer was dried with magnesium sulfate and filtered. The filtrate was conc-entrated under reduced pressure, yielding about 2.9 grams of 3-(2-fluoro-4-hydroxyphenyl)-1-methyl-6-trifluoromethyluracil, mp 185°-190° C. The NMR spectrum was consistent with the proposed structure.

WORKUP

后处理

  1. additionUpon completion of addition
  2. customThe organic layer was separated
  3. extractionthe aqueous layer was extracted with methylene chloride
  4. extractionThe methylene chloride extract
  5. washwashed with water
  6. dry with materialThe organic layer was dried with magnesium sulfate
  7. filtrationfiltered