HRID1995439

反应详情

EQUATION

反应方程式

HRID 1995439 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Hydroxymethyl-6-methyl-4-(3-nitrophenyl)-3-ethoxycarbonyl-5-(β-ethoxyethoxy)carbonyl-1,4-dihydropyridine (420 mg) was dissolved in benzene (20 ml), chlorosulfonyl isocyanate (0.2 ml) was added thereto, and the mixture was reacted under stirring at room temperature for 30 minutes. Water (10 ml) was added to the reaction mixture under cooling, and the mixture was stirred at room temperature for 30 minutes for hydrolysis. The reaction mixture thus obtained was extracted with ethyl acetate, and the extracted solution was washed with water, dried and then concentrated under reduced pressure. The residue was recrystallized from diisopropyl ether/hexane, whereupon crystals (290 mg, yield: 62.6%) were obtained.

WORKUP

后处理

  1. customthe mixture was reacted
  2. temperatureunder cooling
  3. stirringthe mixture was stirred at room temperature for 30 minutes for hydrolysis
  4. customThe reaction mixture thus obtained
  5. extractionwas extracted with ethyl acetate
  6. washthe extracted solution was washed with water
  7. customdried
  8. concentrationconcentrated under reduced pressure