HRID1392554

反应详情

EQUATION

反应方程式

HRID 1392554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5-(2,6-Dibromo-3-methyl-4-nitrophenoxy)-2-hydroxy-3-isopropylbenzaldehyde of Part 8D (100 mg, 0.21 mmol), Na2S2O4 (553 mg, 3.2 mmol), NaHCO3 (0.2 mL, saturated aqueous solution) and ethanol (1.8 mL) were mixed in a microwave safe reaction vial. The vial was sealed and irradiated for 5 minutes at 140° C. NaHCO3 (5 mL, saturated aqueous solution) was added to the reaction mixture and the organic phase removed in vacuo. The obtained suspension was extracted with CHCl3 and the two phases were separated with phase separator (IST). The organic phase was concentrated and filtration through a pad of silica gave 25 mg (27%) of 5-(4-amino-2,6-dibromo-3-methylphenoxy)-2-hydroxy-3-isopropylbenzaldehyde as white foam.

WORKUP

后处理

  1. customThe vial was sealed
  2. customirradiated for 5 minutes at 140° C
  3. customthe organic phase removed in vacuo
  4. extractionThe obtained suspension was extracted with CHCl3
  5. customthe two phases were separated with phase separator (IST)
  6. concentrationThe organic phase was concentrated
  7. filtrationfiltration through a pad of silica