HRID1678269

反应详情

EQUATION

反应方程式

HRID 1678269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

3-Hydroxy-8-nitrobenzo[c]chromen-6-one (Reference Compound No. 1-(2), 52.01 g, 202 mmol) was dissolved in methanol (150 mL)-N,N-dimethylformamide (600 mL), 10% palladium on charcoal (5.00 g) was added thereto, and then the reaction mixture was stirred under hydrogen atmosphere (3 kgf/cm2) at room temperature overnight. After the unsoluble materials were filtered out, the methanol was removed under reduced pressure. Water (2 L) was added to the residue. The precipitated solid was filtered off and dried at 90° C. under reduced pressure to give the titled reference compound (44.02 g) as a pale yellow solid. (Yield 96%)

WORKUP

后处理

  1. additionwas added
  2. filtrationAfter the unsoluble materials were filtered out
  3. customthe methanol was removed under reduced pressure
  4. additionWater (2 L) was added to the residue
  5. filtrationThe precipitated solid was filtered off
  6. customdried at 90° C. under reduced pressure