HRID2242494

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID887

Methanol

CH4O

HCID299600

Methyl 2-[(2-chlorophenyl)methylidene]-3-oxobutanoate

C12H11ClO3

$结构：CCOC(=O)/C=C(\N)COCCN1C(=O)c2ccccc2C1=O$

HCID11174576

未命名化合物

PRODUCTS

生成物

结构：CCOC(=O)C1=C(COCCN2C(=O)c3ccccc3C2=O)NC(C)=C(C(=O)OC)C1c1ccccc1Cl

HCID9871958

Phthalimidoamlodipine

C28H27ClN2O7

收率 69.6%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID3776

Isopropanol

C3H8O

CONDITIONS

反应条件

温度: 0 °C

PROCEDURE

实验过程

Methyl 2-(2-chlorobenzyliden)acetoacetate (40.6 g; 169.9 mmol) was condensed with ethyl 3-amino-4-[2-(phthalimido)ethoxy]crotonate (51.5 g; 161.8 mmol) in 2-propanol (160 ml) under reflux for 11 hours. Methanol (103 ml) was added and mixture was cooled to 5/0° C. The solid was filtered off and dried at 40° C. Phthaloyl Amlodipine (60.7 g, purity: 98.6%; 0.86% of impurity HA) was obtained.

WORKUP

后处理

temperatureunder reflux for 11 hours
filtrationThe solid was filtered off
customdried at 40° C