来曲唑杂质29

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 30.4 g (0.2 mole) of o-cyanobenzyl chloride are dissolved in 70 g of dimethylformamide, and 24 g (0.6 mole) of sodium hydroxide powder are added at the same time as nitrogen is passed in. The mixture is stirred at 20° C. for about 6-10 hours until all the organically bound chlorine has reacted, 70 g of methanol are added dropwise, and the precipitate is filtered off with suction at 0° C. and is washed with methanol and then with water until no chlorine ions are detectable in the water from the wash. Drying gives 17.8 g of stilbene-2,2'-dicarbonitrile in the form of white crystals. has reacted the precipitate is filtered off with suction at 0° C. is washed with methanol Drying

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 450 mg (1.16 mmole) of 4-(4- aminobenzyl)-3-n-butyl-5-(4-chlorobenzylthio)-4H-1,2,4-triazole (Step B), 438 μl (325 mg, 2.52 mmole) of N,N-diisopropylethylamine and 418 mg (2.53 mmole) of 2-cyanobenzyl chloride [R. Scholl and W. Neuberger, Monatsh. Chem. 33, 507 (1911)] in 10 ml of dry THF was stirred overnight at room temperature under N2. The mixture was filtered, and the filtrate was concentrated in vacuo. The residue was dissolved in 50 ml of ethyl acetate and washed with 2×60 ml of saturated NaHCO3 solution followed by 50 ml of saturated NACl. The organic phase was then dried (MgSO4), filtered, and concentrated. A solution of the residue in CH2Cl2 was treated with approximately 2 g of silica gel, and the mixture was evaporated to give a dry powder, which was added as a slurry in hexane to the top of a silica gel column packed in the same solvent. The column was eluted briefly with hexane and then with a stepwise gradient from 1:1 hexane-EtOAc to 100% EtOAc. Two major products were eluted, the second of which correspond to the desired product. Fractions containing this material were combined and concentrated to give 229 mg (36%) of the title compound as a solid, mp 75°-77° C. dec., homogeneous by TLC in 1:3 hexane-EtOAc; mass spectrum (FAB) m/e 516 (M+1)+. The mixture was filtered the filtrate was concentrated in vacuo The residue was dissolved in 50 ml of ethyl acetate washed with 2×60 ml of saturated NaHCO3 solution The organic phase was then dried (MgSO4) filtered concentrated A solution of the residue in CH2Cl2 was treated with approximately 2 g of silica gel the mixture was evaporated to give a dry powder, which The column was eluted briefly with hexane Two major products were eluted Fractions containing this material concentrated

反应条件: temp:20.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 30.4 g (0.2 mole) of o-cyanobenzyl chloride are dissolved in 70 g of dimethylformamide, and 24 g (0.6 mole) of sodium hydroxide powder are added at the same time as nitrogen is passed in. The mixture is stirred at 20° C. for about 6-10 hours until all the organically bound chlorine has reacted, 70 g of methanol are added dropwise, and the precipitate is filtered off with suction at 0° C. and is washed with methanol and then with water until no chlorine ions are detectable in the water from the wash. Drying gives 17.8 g of stilbene-2,2'-dicarbonitrile in the form of white crystals. has reacted the precipitate is filtered off with suction at 0° C. is washed with methanol Drying