The N‟-2- (bromophenyl)-N,N-dimethylurea 16 underwent lithiation on the nitrogen to form a monolithio intermediate using MeLi, followed by bromine-lithium exchange using t-BuLi to give the dilithio species 17. 14 The intermediate 17 was then exposed to carbon monoxide to give 18, which after cyclization forms the intermediate 19, followed by loss of LiNMe2 to give 20, and finally after work up with dilute acid yielded the isatin product 1. 1 13 14 15 6 N O O 1) MeLi, 0 C CO Br N H O NMe2 2) t-BuLi, 0 C Li N O NMe2 Li C N Li O Li O NMe2 N O NMe2 O Li Li -LiNMe2 N H O O Li H3O + X X X X X X A rather versatile and novel two step synthesis of isatins was presented by Mironov in 2001 and allowed for the preparation of isatins containing electron withdrawing groups such as - CF3, -NO2, and -Cl. The method is based on the reaction between aromatic isocyanides and tertiary amines,15 where in the first step, 2-triethylammonio-3-arylaminoindolates 23 were obtained from the corresponding aromatic formamides 21 without isolation of the intermediate isocyanides 22. 16 Heating the 2-triethylammonio-3-arylaminoindolates 23 in excess thionyl chloride followed by hydrolysis led to the target
This helps to indicate whether or not the reaction follows Markovnikov’s Rule, which states that the electrophile (E+) will add to the carbon involved in a double bond that produces the most stable carbocation. If the rule is followed, the reaction will proceed according to the mechanism in Figure 1. In the silver nitrate test, the alkyl bromide is added to AgNO3. The rate of precipitation with 2° should be faster than the solution with the 1° alkyl halide. In the sodium iodide test, the alkyl halide is added to sodium iodide in acetone.
3. Phytochemical Screening and Preliminary Screening for Flavonoids 3.1 Alkaloidal analysis (Preliminary Test) About 20 grams of the sample from the extract were placed in the evaporating dish. It was evaporated over steam bath until syrupy consistency is formed. 5 mL of 2M HCl was added, heated and stirred for about 5 minutes in a water bath and allowed it to cool. 0.5 grams of NaCl was added, stirred and filtered.
In this experiment I set up a lab that examined how 5 different concentrations of HCL (each concentration differing by 5ml of HCL) reacted with CaCO3 and performed three trials for each concentration of HCL, I then found then average of the results and used the averages to form an accurate graph comparing the rate of reaction for each concentration of HCL when mixed with CaCO3 chips. In this experiment I placed 5g of CaCO3 chips in a conical flask and then mixed the different concentrations of HCL with the calcium carbonate. As soon as all of the acid was poured in I attached a delivery tube to the conical flask and watched the CO2 form in upside down graduated cylinder (see diagram). The reaction observed
The graphical illustration of the representative configurations under consideration is depicted in Figure 2. Possible interactions which considered for HOY molecules with HC3OX are including hydrogen bonding (O···H) and halogen bonding (X···Y,O···X) which have been denoted as XYm. The X is representing the cyclopropenone (HC3OF, HC3OCl, HC3OBr, and HC3OI were defined as F, Cl, Br and I, respectively); Y shows the HOY molecules (HOF, HOCl, HOBr, and HOI were defined as F, Cl, Br and I, respectively) and m was applied for displaying the type of complex that formed between them. For example FI1 shows type 1 complex of HC3OF with HOI or BrBr2 is illustrating type 2 complex of HC3OBr with HOBr. The XY1 type shows O···H interactions, which HOY acts as hydrogen bond donor (HBD).
Abstract In this experiment, the reaction kinetics of the hydrolysis of t-butyl chloride, (CH3)3CCl, was studied. The experiment was to determine the rate constant of the reaction, as well as the effects of solvent composition on the rate of reaction. A 50/50 V/V isopropanol/water solvent mixture was prepared and 1cm3 of (CH3)3CCl was added. At specific instances, aliquots of the reaction mixture were withdrawn and quenched with acetone. In addition, phenolphthalein was added as an indicator.
Regarding reaction 4, the duration was changed to 480 seconds. After the Styrofoam cups were restacked, 100mL HCl was added. The lid was added and the probe was instered. A watch glass was weighed, then weighed again after scooping on 1.0g MgO. After 3-4 readings were recorded, the MgO was added with the spatula, which was stirred constantly with the stir bar.
5 mL of the sample tempered at 20 oC is taken by the pipette in the cuvette for the centrifugation. 0,2 mL 6 mol/dm3 of hydrochloric acid and 10 mL iso-octane (2,2,4-trimethylpentane) is added to the cuvette for the centrifugation, and shaken for 15 minutes in the shaker, and then centrifuged for 10 minutes at 3000 rounds per minute. The absorbance of the iso-octane extract is measured on the spectrophotometer at 275 nm in cuvette of 1 cm, with respect to the blank test which was the iso-octane of the same quality. The programmed method for the bitterness of the beer caused the calculated values on the spectrophotometer by the following formula: The standard values for the beer are 10-40 BU, depending on sort, type and origin. Total polyphenols (EBC method) The method is based on the fact that, in alkaline medium, polyphenols react with iron (III) ions with the formation of the colored compexes, and the obtained brown colout is measured spectrophotometrically.
Solubility: The solubility of the drug sample was carried out in different solvents (aqueous and organic) according to I.P. The results are then compared with those mentioned in the official books and Indian Pharmacopoeia. Melting point The melting point of Itraconazole was determined by capillary method using digital melting point apparatus. ANALYTICAL METHODS STANDARD CURVE Preparation of standard solution: 100mg of itraconazole was accurately weighed into 100ml volumetric flask and dissolved in small quantity of buffer. The volume was made with 6.8 pH Phosphate buffer to get a concentration of 1000µg/ml (SS-I).