HRID1829002

反应详情

EQUATION

反应方程式

HRID 1829002 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 3-(6-Amino-3H-isobenzofuran-1-ylidene)-1,3-dihydro-indol-2-one (25.0 mg, 0.095 mmol), 3-bromo-1-propanol (85.5 μL, 0.946 mmol), and silver sulfate (59.0 mg, 0.189 mmol) in 0.8 mL DMF was heated at 120° C. for 1.5 h. The mixture was partitioned between EtOAc and H2O and the organic layer separated from the silver salts. The solution was washed with H2O, brine and then dried with Na2SO4. Concentrating the solution in vacuo gave a residue which was purified by chromatography (silica gel, CHCl3/MeOH, 96:4) to give the title compound (3 mg, 10%) as a yellow solid.

WORKUP

后处理

  1. customThe mixture was partitioned between EtOAc and H2O
  2. customthe organic layer separated from the silver salts
  3. washThe solution was washed with H2O, brine
  4. dry with materialdried with Na2SO4
  5. concentrationConcentrating the solution in vacuo
  6. customgave a residue which
  7. customwas purified by chromatography (silica gel, CHCl3/MeOH, 96:4)