HRID732250

反应详情

EQUATION

反应方程式

HRID 732250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (0.13 mL) was added to a mixture of 5,6-diethoxy-7-fluoro-2,3-dihydroisoindol-1-ylideneamine sulfate (225 mg, 0.67 mol) produced in Example 2, water (2.3 mL) and toluene (2.3 mL). The mixture was stirred at room temperature. After the layers were separated, the organic layer was re-extracted with water (1.2 mL), the aqueous layers were combined, and a 5N aqueous solution of sodium hydroxide (0.3 mL) was added thereto on ice. The mixture was stirred on ice, and then precipitated crystals were filtered and dried at room temperature under reduced pressure to give 133 mg of the title compound (yield: 84%) as grayish white crystals.

WORKUP

后处理

  1. customAfter the layers were separated
  2. extractionthe organic layer was re-extracted with water (1.2 mL)
  3. additiona 5N aqueous solution of sodium hydroxide (0.3 mL) was added
  4. stirringThe mixture was stirred on ice
  5. customprecipitated crystals
  6. filtrationwere filtered
  7. customdried at room temperature under reduced pressure