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HRID1111454

反应详情

EQUATION

反应方程式

HRID 1111454 的结构方程式

REACTANTS

反应物

3
结构：C1CCC2=NCCCN2CC1
HCID81184

1,8-Diazabicyclo[5.4.0]undec-7-ene

C9H16N2

结构：COc1c(F)c(F)cc2c(=O)c(C(=O)O)cn(C3CC3)c12
HCID7019465

1-Cyclopropyl-6,7-difluoro-8-methoxy-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

C14H11F2NO4

结构：CNCC1CCNC1
HCID13491795

N-Methyl-1-(pyrrolidin-3-yl)methanamine

C6H14N2

PRODUCTS

生成物

1
结构：CNCC1CCN(c2c(F)cc3c(=O)c(C(=O)O)cn(C4CC4)c3c2OC)C1
HCID483413

1-Cyclopropyl-6-fluoro-8-methoxy-7-{3-[(methylamino)methyl]pyrrolidin-1-yl}-4-oxo-1,4-dihydroquinoline-3-carboxylic acid

C20H24FN3O4

收率 49.3%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC#N
溶剂HCID6342

Acetonitrile

C2H3N

PROCEDURE

实验过程

A mixture of 1-cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid (200 mg), 3-methylaminomethylpyrrolidine (90 mg), DBU (110 mg) and anhydrous acetonitrile (3 ml) was refluxed for 75 minutes. After cooling, the resulting precipitate was collected by filtration and recrystallized from a solution of dichloromethane-methanol (1:1) to give the title compound (130 mg) as white powdery crystals, mp 226.5°-230° C.

WORKUP

后处理

  1. temperaturewas refluxed for 75 minutes
  2. temperatureAfter cooling
  3. filtrationthe resulting precipitate was collected by filtration
  4. customrecrystallized from a solution of dichloromethane-methanol (1:1)