A mixture of compound 5 (2.0 g, 9.97 mmol), trimethylsilyl cyanide (2.5 mL, 19.95 mmol) and diethylcarbamoyl chloride (2.75 mL, 29.92 mmol) in anhydrous acetonitrile (3 mL) was irradiated at 100°C (80 W, Milestone Start E) for 1 h. Upon cooling, the mixture was poured into crushed ice and extracted with dichloromethane. The combined organic layers were dried over sodium sulfate and evaporated to dryness. The crude product was purified by column chromatography (silica gel) using a mixture of cyclohexane / ethyl acetate (1/1, v/v) as the eluent to provide pure 6 (1.8 g, 87%). Mp 174–6°C (EtOAc). 1H NMR (600 MHz, acetone-d6) δ 9.21 (brs, 1H, D2O exch, NH), 7.91 (s, 1H, H-5), 2.39 (s, 3H, 4-CH3), 2.23 (s, 3H, COCH3) 13C NMR (151 MHz, acetone-d6) δ 169.4 (CO), 153.0 (C-2), 141.0 (C-4), 134.0 (C-3), 130.0 (C-6), 129.9 (C-5), 115.8 (CN), 23.1 (COC H3), 17.2 (4-CH3). HR-MS (ESI) m/z: Calcd for C9H9ClN3O: [M1+H]+ = 210.0429, found 210.0431. Anal. Calcd for C9H8ClN3O: C, 51.57; H, 3.85; N, 20.05. Found: C, 51.39; H, 3.73; N, 20.22.
Start e
Manufactured by Milestone
Sourced in Italy
Start E is a versatile lab equipment product designed for various applications in research and laboratory settings. Its core function is to provide a stable and reliable platform for the precise measurement and analysis of samples.
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Lab products found in correlation
4 protocols using start e
1
Synthesis of 4-Acetyl-2-Chloro-6-Methylpyridine-3-Carbonitrile
2
Brain Tissue Heavy Metal Analysis
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Ten animals per group were anesthetized with ketamine hydrochloride (90 mg/kg) and xylazine hydrochloride (9 mg/Kg), the brains removed from the cranial box and the structures rapidly dissected in cold places and frozen in liquid nitrogen, kept in ultra-freezer (−80 °C) until the moment of analysis. Subsequently, the tissues were lyophilized. After lyophilization, as the amount of mass obtained was small, a pool of samples per group was performed. A mass of each sample was weighed and transferred to the digestion bottle, adding 4.0 mL HNO3 (14 mol/L), 2.0 mL H2O2 (35% w/w), and 2.0 mL ultrapure H2O. The digestion of the samples was performed in triplicate, in a microwave oven with a cavity (START E, Milestone, Sorisole, Italy) at a temperature of 180 °C and power of 800 W, for 25 min.
After digestion, the solutions were transferred to volumetric vials, maintaining a final volume of 40 μL with ultrapure water. For Pb determination, the samples were diluted to the final acidity of 5.0%.
After digestion, the solutions were transferred to volumetric vials, maintaining a final volume of 40 μL with ultrapure water. For Pb determination, the samples were diluted to the final acidity of 5.0%.
3
Determination of Aluminum Concentration
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A lyophilizer (Model L101, Liotop, Sao Carlos, SP, Brazil) was used for drying the samples. After drying, the samples were pulverized with a mortar and pestle. Acid digestion of samples was performed in a microwave oven (Start E, Milestone, Sorisole, Italy) [20 (link)]. Determinations of the total concentration of Al in the digested samples were carried out using a Varian Spectra AA 240Z atomic absorption spectrometer (Mulgrave, Victoria, Australia) equipped with a transverse Zeeman effect background corrector and a longitudinal-heated graphite furnace atomizer. An Al hollow cathode lamp was employed as a radiation source, operating at 10 mA. Absorbance signals were measured using the 256.8 nm line at a spectral resolution of 0.5 nm. All measurements were based on integrated absorbance. Argon (99.999% purity, Linde, Pará, Brazil), was used as the purge gas. The temperature programs used for determination Al in samples are shown in Table 1 .
4
Microwave Digestion of Tree Ring Samples
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Sample discs were sawn to a thickness of approximately 0.5 cm. For the analysis with LA-ICP-MS, a part of sample near the previously burned line was taken from different rings. For each tree ring two samples were prepared. Weight of samples varied between 0.2 and 0.5 g. Samples were transferred to digestion vessels of microwave furnaces. Six mL of concentrated HNO3 and 2 mL of concentrated H2O2 were added directly to each sample, and samples were digested by means of closed-vessel microwave-assisted digestion (Start E ® , Mile-stone, Shelton, CT, USA). Digestion temperature was raised to 150 °C in 15 min, and then held for another 30 min. Digested samples were transferred to 25 mL volumetric flasks and diluted with deionised water until mark.
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