HRID604285

反应详情

EQUATION

反应方程式

HRID 604285 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At room temperature, a solution of 2-Bromomethyl-3-methoxy-6-nitro-benzoic acid methyl ester (crude 7.0 g, 18.2 mmol) in 46 mL of THF is treated with 2M solution of methylamine in THF (27.3 mL, 54.6 mmol), and the mixture is stirred for 4 hours at the room temperature. The reaction mixture is quenched with a saturated ammonium chloride solution and partitioned between ethyl acetate. The organic layer is washed with brine and then dried over Na2SO4 following concentrated to give 4-Methoxy-2-methyl-7-nitro-2,3-dihydro-isoindol-1-one (3.1 g) as orange solid in 77% yields (2 steps). 1H-NMR (400 MHz, δ, ppm) CDCl3: 3.19 (s, 3H), 3.99 (s, 3H), 4.32 (s, 2H), 7.0 (d, 1H), 7.89 (d, 1H).

WORKUP

后处理

  1. customThe reaction mixture is quenched with a saturated ammonium chloride solution
  2. custompartitioned between ethyl acetate
  3. washThe organic layer is washed with brine
  4. dry with materialdried over Na2SO4 following
  5. concentrationconcentrated