反応 #1996

反応方程式

product

1-cyclopropyl-8-(1-hydroxycarbonyl-1-cyclopropyl)-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid ethyl ester

diphenylphosphoryl azide

t-butanol

triethylamine

→

1-cyclopropyl-8-(1-Bocamino-1-cyclopropyl)-7-fluoro-9-methyl-4-oxo-4H-quinolizine-3-carboxylic acid ethyl ester

溶媒

dioxane

反応条件

後処理

1. 1
   その他The solvents is removed under vacuum
2. 2
   workup.DISSOLUTIONThe residue is dissolved in methylene chloride
3. 3
   洗浄washed with water
4. 4
   乾燥dried over MgSO4
5. 5
   濃縮concentrated under vacuum
6. 6
   その他The title compound is purified by chromatography on silica gel

実験手順

A sample of the product from Step 477d is heated with diphenylphosphoryl azide, t-butanol, triethylamine and dioxane. The solvents is removed under vacuum. The residue is dissolved in methylene chloride, washed with water and dried over MgSO4 and concentrated under vacuum. The title compound is purified by chromatography on silica gel.

出典