تفاعل #64442

معادلة التفاعل

Ethenylidenebisphosphonic acid tetraethyl ester

1-phenyl-2-(2-pyridinyl)ethanone

N-(6-methoxybenzothiazol -2-yl)-3-oxo-3-phenylpropanamide

potassium carbonate

→

title compound

[4-Oxo4-phenyl-3-(2-pyridinyl)butylidene]bisphosphonic acid tetraethyl ester hemihydrate

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   تركيزThe reaction is concentrated under reduced pressure
2. 2
   غسيلwashed with sodium chloride
3. 3
   تجفيفdried with magnesium sulfate
4. 4
   تركيزconcentrated under reduced pressure
5. 5
   أخرىThe product is chromatographed
6. 6
   غسيلeluting with ethyl acetate
7. 7
   تركيزconcentrated

الإجراء التجريبي

Ethenylidenebisphosphonic acid tetraethyl ester (I, 3.00 g), 1-phenyl-2-(2-pyridinyl)ethanone (II, 2.17 g) and potassium carbonate (2.07 g) are stirred in methanol (20 ml) overnight. The reaction is concentrated under reduced pressure, taken up in ethyl acetate, washed with sodium chloride, dried with magnesium sulfate, and concentrated under reduced pressure. The product is chromatographed eluting with ethyl acetate. The appropriate fractions are pooled and concentrated to give the title compound, MS (m/e) 497, 452, 392, 302 and 288; IR (neat) 2983, 1683, 1597, 1580, 1470, 1448 and 1253 cm-1 ; NMR (CDCl3) 8.52, 8.02, 7.60, 7.49, 7.37, 7.11, 5.46, 4.12, 2.75, 2.55, 1.36, 1.25 and 1.16 δ.

المصدر