HRID1844005

反应详情

EQUATION

反应方程式

HRID 1844005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-(4-Methoxybenzyl)-3,4-dihydro-2,7-naphthyridin-1(2H)-one (I-65e: 700 mg, 2.6089 mmol) and p-toluene sulphonic acid (1.985 g, 10.436 mmol) in toluene (15 mL) were refluxed for 6 hours. The reaction was monitored by TLC (10% methanol in CHCl3). The reaction mass was neutralized with sodium carbonate solution, distilled off the solvent and added 10% methanol in CHCl3. The solid precipitated was filtered and distilled off the solvent to afford the crude product. Purification by column chromatography on silica gel (7% methanol in DCM) afforded 280 mg of the product (72.53% yield).

WORKUP

后处理

  1. distillationdistilled off the solvent
  2. additionadded 10% methanol in CHCl3
  3. customThe solid precipitated
  4. filtrationwas filtered
  5. distillationdistilled off the solvent
  6. customto afford the crude product
  7. customPurification by column chromatography on silica gel (7% methanol in DCM)