تفاعل #1584

معادلة التفاعل

isopropyl 3-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]-pyridazin-1-ylidene)amino]phenyl}tetrahydro-2,4,6-trioxo-s-triazine-1(2H)-acetate

potassium carbonate

isopropyl bromoacetate

water

→

title product

المردود 29.5%

Diisopropyl 5-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H, 3H-[1,3,4 ]thiadiazolo[3,4-a]pyridazin-1-ylidene) amino]phenyl}dihydro-2,4,6-trioxo-s-triazine-1,3 (2H,4H)-diacetate

المردود 29.5%

المذيبات

N,N-dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   استخلاصThe aqueous mixture is extracted with ethyl acetate
2. 2
   استخلاصThe organic extract
3. 3
   غسيلis washed with brine
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   تركيزconcentrated in vacuo
6. 6
   أخرىto obtain an orange gel

الإجراء التجريبي

A mixture of isopropyl 3-{2-chloro-4-fluoro-5-[(tetrahydro-3-oxo-1H,3H-[1,3,4]thiadiazolo[3,4-a]-pyridazin-1-ylidene)amino]phenyl}tetrahydro-2,4,6-trioxo-s-triazine-1(2H)-acetate (0.85 g, 1.62 mmol), potassium carbonate (0.27 g, 1.95 mmol) and isopropyl bromoacetate (0,353 g, 1.95 mmol)in N,N-dimethylformamide is stirred overnight at room temperature and poured into water. The aqueous mixture is extracted with ethyl acetate. The organic extract is washed with brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain an orange gel. Flash column chromatography of the gel using silica gel and an ethyl acetate/hexanes solution (2:3) gives the title product as a yellow gel (0.3 g) which is identified by NMR spectral analysis.

المصدر