反応 #1584

反応方程式

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

収率 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

収率 29.5%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   抽出The aqueous mixture is extracted with ethyl acetate
2. 2
   抽出The organic extract
3. 3
   洗浄is washed with brine
4. 4
   乾燥dried over anhydrous magnesium sulfate
5. 5
   濃縮concentrated in vacuo
6. 6
   その他to obtain an orange gel

実験手順

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.

出典