HRID1162033

反应详情

EQUATION

反应方程式

HRID 1162033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chlorosulphonic acid (43.4 g, 0.366 mol) in DCM (10 mL) was added to a cold solution (5° C.) of 2,3-dihydrobenzofuran (20 g, 0.166 mol) in DCM (200 mL). After the addition the reaction was left with stirring at room temperature overnight. The reaction mixture was quenched with water (150 mL) keeping the temperature below 10° C. The organic phase was separated and washed with an aqueous solution of NaHCO3 (13.9 g dissolved in 150 mL of water). The organic solvents were evaporated to yield the title compound as a solid residue 3.3 g (23%). 1H NMR 270 MHz (CDCl3) δ ppm 3.32 (t, J=8.91 Hz, 2H) 4.75 (t, J=8.91 Hz, 2H) 6.90 (d, J=9.15 Hz, 1H) 7.78-7.90 (m, 2H)

WORKUP

后处理

  1. additionAfter the addition the reaction
  2. waitwas left
  3. customThe reaction mixture was quenched with water (150 mL)
  4. customthe temperature below 10° C
  5. customThe organic phase was separated
  6. washwashed with an aqueous solution of NaHCO3 (13.9 g dissolved in 150 mL of water)
  7. customThe organic solvents were evaporated