تفاعل #44960

معادلة التفاعل

t-butanol

2-{[(5-Chloropyridin-2-yl)amino]carbonyl}-3-({[trans-4-(3-oxomorpholin-4-yl)cyclohexyl]carbonyl}amino)furo[3,2-b]pyridine-5-carboxylic acid

triethylamine

diphenylphosphoryl azide

→

title compound

t-Butyl [2-{[(5-chloropyridin-2-yl)amino]carbonyl}-3-({[trans-4-(3-oxomorpholin-4-yl)cyclohexyl]carbonyl}amino)furo[3,2-b]pyridin-5-yl]carbamate

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction solution is concentrated under reduced pressure
2. 2
   workup.ADDITIONThe residue is diluted with chloroform
3. 3
   غسيلwashed with water and saturated brine
4. 4
   تجفيفThe organic layer is dried over sodium sulfate
5. 5
   أخرىthe solvent is evaporated under reduced pressure
6. 6
   أخرىThe resulting residue is purified by silica gel column chromatography (eluent: chloroform/methanol=100/1 followed by 20/1)

الإجراء التجريبي

2-{[(5-Chloropyridin-2-yl)amino]carbonyl}-3-({[trans-4-(3-oxomorpholin-4-yl)cyclohexyl]carbonyl}amino)furo[3,2-b]pyridine-5-carboxylic acid (6.80 g) obtained in Example 79 is suspended in t-butanol (300 ml). To the suspension are added triethylamine (3.48 ml) and diphenylphosphoryl azide (5.39 ml) at room temperature, and the mixture is stirred at 100° C. for 15 hours. The reaction solution is concentrated under reduced pressure. The residue is diluted with chloroform, and washed with water and saturated brine. The organic layer is dried over sodium sulfate, and the solvent is evaporated under reduced pressure. The resulting residue is purified by silica gel column chromatography (eluent: chloroform/methanol=100/1 followed by 20/1) to give the title compound (5.64 g).

المصدر