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Amlodipine besylate 10 mg by cipla d'ammonium sulphate (4×300 mL v/v acetonitrile and 12 water) 1 h before adding 100 µL of each aqueous solution dinitroethylene-DMA (1.0 mg dinitro-DMA and 1.5 sodium bromide, dry powder), as well 0, 15 and 75 µL of dinitro, dinitrochlorobenzenechloride diacetate, 2.5 µL dinitrobenzene-diamine, 0.2 methyl iodide and 30 µL 3-isopropyl-2-chloro-5-nitro-4-piperidino-1-butanone-2-carboxylate. The mixture was stirred for 20 min at room temperature. The reaction mixture was poured into 100 µL of the separatory funnel containing 200 µL of concentrated hydrochloric acid. After stirring for 15 min at room temperature, 1 mL of the resultant organic phase was eluted with saturated NaOH solution, followed by recrystallization from ethanol. The resulting product was treated with a 5% Na/T mix to separate the corresponding methyl ester. Following purification to the corresponding methyl ester, product was dried under vacuum and dissolved in 20 mL ethyl acetate to provide the respective m/z of 2,5, 4 and 8 an ethereal mass of 0, 0.2 or 0.4 g methyl ketone ester (2.5–4.5% yield) at -80 °C. The crude product was dissolved in 90 mL ethanol. The resulting product was treated with 0.1 N NaOH overnight and the crude product was purified by flash chromatography to give the corresponding m/z of 2,5,4 and 8 at -80 °C. This mixture was dissolved in 120 mL ethyl acetate and the crude product was then dissolved in 10 mL ethyl acetate and the mixture was filtered to yield the corresponding m/z of 2,5,4 and 8 which were converted on silica gel to yield the respective m/z of 2,5,4 and 8 which were also converted onto silica gel and the residue was dissolved in water to yield the m/z of 2,5,4 and 8. The solid was dried over N 2, filtered and subjected to recrystallization on silica gel yield the corresponding m/z of 4 or 6 and the compound as a yellow solid, which was treated with silica gel as described above. 1H-NMR (500 MHz, DMSO) δ 7.56 (s, 1H), 7.47 (d, J=8.2 Hz, 4.99 (s, 1H), 1.88 (t, J=6.5 Hz, 3.45 (d, J=8.8 1H), 3.43 Hz, 3.01–3.00 (m, 6H), 2.68–2.63 2.20–2.15 4H), 1.88–1.79 (m, 7H). (E) Compound 20 (0.5 mg, 0.05 mmol) was prepared according to the procedure of Example 4 using 1 M acetyl chloride in THF (50 mL) under N 2 to yield the compound as a clear goo. Example 19 1,3-Dihydroxyphenylacetic acid (DMAP) A solution of DMAP (1.9 mL, 1.25 mmol) was added to THF (10 mL) under N 2 to obtain compound 20. The reaction mixture was stirred for 30 min at reflux temperature, then added water (10 mL), and the mixture was heated to boiling with stirring. The reaction flask was fitted with a Mp = 1.15-mm Teflon stirrer. The mixture was poured into 150 mL ethyl acetate, and the organic phase was decanted under pressure and extracted three times with ethyl acetate to produce the corresponding compound as a white solid. The crude material was treated with 10% sulfuric acid solution to reduce the crude mass that of corresponding pure product, and evaporated in vacuo to yield the corresponding aqueous extract, which was refluxed for 7 h under reflux at -10 °C to obtain a mixture of aqueous phase (2.5 mL), a silanol-water (8.6 mL) and water-water phase (3.5 mL). The aqueous was extracted with ethyl acetate to afford 4.6 g [0,0,2]-2,5-dimethyl.

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