HRID2302250

反应详情

EQUATION

反应方程式

HRID 2302250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thiophene-2-carbonyl chloride (0.069 g) was added to a stirred suspension of N-(3-amino-4-methylphenyl)-3-morpholinobenzamide (0.104 g), triethylamine (0.15 ml) and methylene chloride (20 ml) and the resultant mixture was stirred at ambient temperature for 4 hours. The organic phase was washed with water and with a saturated aqueous sodium bicarbonate solution, dried (MgSO4) and evaporated. The residue was dissolved in methylene chloride (2 ml) and diethyl ether (20 ml) was added to give a precipitate which was isolated by filtration, washed with diethyl ether and dried. There was thus obtained the title compound (0.047 g); NMR Spectrum: (DMSOd6) 2.18 (t, 3H), 3.18 (t, 4H), 3.76 (t, 4H), 7.14 (d, 1H), 7.20 (m, 2H), 7.38 (m, 2H), 7.41 (s, 1H), 7.58 (m, 1H), 7.78 (s, 1H), 7.82 (d, 1H), 7.98 (d, 1H), 9.93 (s, 1H), 10.13 (s, 1H); Mass Spectrum: M+H+ 422.

WORKUP

后处理

  1. washThe organic phase was washed with water and with a saturated aqueous sodium bicarbonate solution
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. dissolutionThe residue was dissolved in methylene chloride (2 ml)
  5. additiondiethyl ether (20 ml) was added
  6. customto give a precipitate which
  7. customwas isolated by filtration
  8. washwashed with diethyl ether
  9. customdried