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HRID4658

反应详情

EQUATION

反应方程式

HRID 4658 的结构方程式

REACTANTS

反应物

3
结构：COC(=O)CC(C)=O
HCID7757

Methyl acetoacetate

C5H8O3

结构：COC(=O)/C=C(/C)N
HCID643918

2-Butenoic acid, 3-amino-, methyl ester, (2Z)-

C5H9NO2

结构：CS(=O)(=O)c1ccc(OCCCCBr)c(C=O)c1
HCID14050491

未命名化合物

PRODUCTS

生成物

1
结构：COC(=O)C1=C(C)NC(C)=C(C(=O)OC)C1c1cc(S(C)(=O)=O)ccc1OCCCCBr
HCID14050492

未命名化合物

收率 53%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)O
溶剂HCID3776

Isopropanol

C3H8O

PROCEDURE

实验过程

7.6 g of 2-(4-bromobutoxy)-5-methylsulfonylbenzaldehyde, 2.6 g of methyl acetoacetate and 2.9 g of 3-aminocrotonic acid methyl ester were dissolved in 16 ml of isopropanol, and the solution was heated for 5 hours. After cooling, precipitated crystals were collected by filtration, and recrystallized from methanol to give 6.3 g of dimethyl 4-[2(4-bromobutoxy)-5-methylsulfonylphenyl]-2,6-dimethyl-1,4-dihydropyridine-3,5-dicarboxylate.

WORKUP

后处理

  1. temperaturethe solution was heated for 5 hours
  2. temperatureAfter cooling
  3. customprecipitated crystals
  4. filtrationwere collected by filtration
  5. customrecrystallized from methanol