反应详情

To a solution of 2-[1-(tert-butoxycarbonyl)-imidazol-4-yl]acetic acid (45 mg) and tetraethyl (aminomethylene)bis(phosphonate) (91 mg) in N,N-dimethylformamide (1 ml) was added N-ethyl-N'-(3-dimethylaminopropyl)carbodiimide hydrochloride (42 mg) with stirring on ice-sodium chloride bath under nitrogen atmosphere. After stirring for 36 hours at 5° C., the mixture was diluted with chloroform (10 ml) and washed with cold 1N aqueous solution of citric acid (10 ml). The aqueous layer was extracted with chloroform (10 ml) twice and the combined organic layers were dried over sodium sulfate and evaporated in vacuo. The residue was dissolved in ethyl acetate (10 ml) and the solution was washed with water (10 ml), dried over sodium sulfate and evaporated in vacuo to give a colorless syrup of tetraethyl [[2-{1-(tert-butoxycarbonyl)-imidazol-4-yl}acetamido]methylene]bis(phosphonate) (67 mg).

1. stirringAfter stirring for 36 hours at 5° C.
2. washwashed with cold 1N aqueous solution of citric acid (10 ml)
3. extractionThe aqueous layer was extracted with chloroform (10 ml) twice
4. dry with materialthe combined organic layers were dried over sodium sulfate
5. customevaporated in vacuo
6. dissolutionThe residue was dissolved in ethyl acetate (10 ml)
7. washthe solution was washed with water (10 ml)
8. dry with materialdried over sodium sulfate
9. customevaporated in vacuo