تفاعل #88406

معادلة التفاعل

sodium hydroxide

Thionyl chloride

2,2,2-trifluoro-1-phenylethanone

2-aminopyridine-4-carboxylic acid methyl ester

→

title compound

المردود 27.7%

(Z)-methyl 2-((2,2,2-trifluoro-1-phenylethylidene)amino)isonicotinate

المردود 27.7%

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   استخلاصthe mixed solution was then extracted with ethyl acetate
2. 2
   تجفيفthe gathered organic layer was then dried over anhydrous sodium sulfate
3. 3
   workup.DISTILLATIONAfter that, the solvent was distilled away under reduced pressure
4. 4
   أخرىThe obtained residue was purified by silica gel column chromatography (silica gel: eluent; heptane:ethyl acetate=2:1-1:1)

الإجراء التجريبي

Thionyl chloride (2.2 ml) was added at 0° C. to a pyridine (4.8 ml) solution of 2,2,2-trifluoro-1-phenylethanone (5.1 g) and 2-aminopyridine-4-carboxylic acid methyl ester (4.5 g). The temperature of the reaction solution was increased to room temperature, and the reaction solution was then stirred for 1 hour. Thereafter, the reaction solution was poured into a 1 N sodium hydroxide aqueous solution, and the mixed solution was then extracted with ethyl acetate. Organic layers were gathered, and the gathered organic layer was then dried over anhydrous sodium sulfate. After that, the solvent was distilled away under reduced pressure. The obtained residue was purified by silica gel column chromatography (silica gel: eluent; heptane:ethyl acetate=2:1-1:1), so as to obtain the title compound (2.5 g) in the form of a yellow liquid.

المصدر