HRID1421850

反应详情

EQUATION

反应方程式

HRID 1421850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoroacetic acid (50 mL) was stirred and cooled in an ice-water bath. To this was added t-butyl N-(6-fluoro-3-methyl-1,2(2H)-benzisoxazol-7-yl)carbamate (3.0 g). Upon completion of addition, the reaction mixture was stirred for one hour and then concentrated to a residue. The residue was taken up in water and made basic to pH 8 with sodium bicarbonate. The mixture was then extracted thoroughly with methylene chloride. The combined extracts were washed with water, dried with magnesium sulfate, and concentrated, yielding 2.1 grams of 7-amino-6-fluoro-3-methyl-1,2(2H)-benzisoxazole. The NMR spectrum was consistent with the proposed structure.

WORKUP

后处理

  1. temperaturecooled in an ice-water bath
  2. additionUpon completion of addition
  3. concentrationconcentrated to a residue
  4. extractionThe mixture was then extracted thoroughly with methylene chloride
  5. washThe combined extracts were washed with water
  6. dry with materialdried with magnesium sulfate
  7. concentrationconcentrated