* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Reference:
[1] Organic Letters, 2011, vol. 13, # 15, p. 3794 - 3797
[2] Asian Journal of Chemistry, 2014, vol. 26, # 3, p. 634 - 640
[3] Journal of the American Chemical Society, 2018, vol. 140, # 6, p. 2062 - 2066
2
[ 5036-02-2 ]
[ 14769-73-4 ]
[ 14769-74-5 ]
Yield
Reaction Conditions
Operation in experiment
39 % ee
With O,O'-dibenzoyl-L-tartaric acid In dichloromethane; water at 40℃; Sonication; Irradiation
We have used equal amounts for these experiments as well.4.08 g (20 mmol) (RS)-TET was dissolved in 10 ml dichloromethaneand 8 ml water at 40 °C and 2.365 g (6.6 mmol) (R,R)-DBTA in14 ml dichloromethane at 40 °C as well. When the solutions wereadded together, ultrasonic irradiation and cooling (5 °C) wasstarted straightaway.We used a Bandelin Sonopuls HD 2200 ultrasonichomogenizer equipped with MS 72 booster horn probe(diameter 2 mm, length 191 mm; shape: exponential taper; resonancefrequency of the equipment is 20 kHz). The sonotrode wasplaced at the same location during the runs: in a vertical positionwith its tip on the water–dichloromethane phase interface. Thetemperature was controlled throughout the whole experiment toavoid the warming effect of ultrasound. The duration of sonicationwas varied between 1, 5, 10, 20 and 30 min. Then we filtered thediastereomeric salt and washed with 1 ml distiled water (Fig. 2).The salt was analysed with chiral reverse-phase HPLC. We used differentultrasonic power and the real power was measured by thecalorimetric method.
Stage #1: With sodium metabisulfite; pyrographite In isopropyl alcohol for 0.5 h;
In 1000 ml four-mouth bottle into L-tetramisole 50g, inputs isopropanol 500g, heating is dissolved, add activated carbon 0.5g, sodium metabisulfite 0.75g stirring decolourizations 30 minutes, filtration, filtrate hydrogen chloride gas under stirring 9g, to pH4-5, filtering, levamisole hydrochloride dried to get 54.3g,yield 92.1percent, the target product without yellow block, long-term storage quality and stability.
With O,O'-dibenzoyl-L-tartaric acid; In dichloromethane; water; at 40.0℃;Sonication; Irradiation;
We have used equal amounts for these experiments as well.4.08 g (20 mmol) (RS)-TET was dissolved in 10 ml dichloromethaneand 8 ml water at 40 C and 2.365 g (6.6 mmol) (R,R)-DBTA in14 ml dichloromethane at 40 C as well. When the solutions wereadded together, ultrasonic irradiation and cooling (5 C) wasstarted straightaway.We used a Bandelin Sonopuls HD 2200 ultrasonichomogenizer equipped with MS 72 booster horn probe(diameter 2 mm, length 191 mm; shape: exponential taper; resonancefrequency of the equipment is 20 kHz). The sonotrode wasplaced at the same location during the runs: in a vertical positionwith its tip on the water-dichloromethane phase interface. Thetemperature was controlled throughout the whole experiment toavoid the warming effect of ultrasound. The duration of sonicationwas varied between 1, 5, 10, 20 and 30 min. Then we filtered thediastereomeric salt and washed with 1 ml distiled water (Fig. 2).The salt was analysed with chiral reverse-phase HPLC. We used differentultrasonic power and the real power was measured by thecalorimetric method.
Formazan/Levamisole Salt 0.1N Sodium hydroxide (13 ml) was added to levamisole hydrochloride (0.33 gram; 0.0014 mole) in 10 ml of water. The free levamisole was extracted into 20 ml of methylene chloride, washed once with water, and dried over magnesium sulfate.
Thus, another embodiment of the present invention is a salt of one or these four compounds with an anthelmintic base selected from the group consisting ofbephenium,diethylcarbamazine,levamisole,morantel,nicotine,piperazine, andpyrantel.
14. and at least one number selected from the group consisting of...IndomethacinNicotinamideDiazepamDisodium chromoglycateLevamisoleAldosteroneNigroglycerineAmyl nitrate...
The solid is refluxed with 2 g of phosphorous pentasulfide in toluene for 20 hours. Toluene is removed under reduced pressure, the residue taken up in 100 ml of chloroform and 100 ml. of 20 percent sodium hydroxide. The organic layer is separated, washed and concentrated to give an oil. This oil is taken in 20 ml of concentrated hydrochloric acid and the solution is refluxed for 1 hour. The solution is cooled, filtered and filtrate made basic with ammonium hydroxide. The mixture is extracted with 2*50 ml of methylene chloride. The combined organic layer is washed, dried and the solvent removed to give an oil which crystallizes on standing. The spectral characteristics are identical to that of tetramisole and the material had a specific rotation [alpha]D20 = -17.7° (c7 in chloroform) corresponding to a 21percent enantiomeric excess of levamisole.
12
[ 15663-27-1 ]
[ 14769-73-4 ]
silver nitrate[ No CAS ]
Pt(2+)*2NH3*C11H12N2S*Cl(1-)*NO3(1-)=[Pt(NH3)2(C11H12N2S)Cl](NO3)[ No CAS ]
In 1000 ml four-mouth bottle into L-tetramisole 50g, inputs isopropanol 500g, heating is dissolved, add activated carbon 0.5g, sodium metabisulfite 0.75g stirring decolourizations 30 minutes, filtration, filtrate hydrogen chloride gas under stirring 9g, to pH4-5, filtering, levamisole hydrochloride dried to get 54.3g,yield 92.1percent, the target product without yellow block, long-term storage quality and stability.