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methyl 2,6-dichloro-4-(3-phenylpyrrolidin-1-yl)benzoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
47.02%
With tris-(dibenzylideneacetone)dipalladium(0); caesium carbonate; 2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl; In toluene; at 110℃; for 16.0h;
To a solution of 0190-1 (2.00 g, 7.41 mmol) and CI (1.05 g, 7.41 mmol) in DMF (5 mL), was added K2CO3 (1.54 g, 11.11 mmol) and the mixture was stirred at room temperature for overnight. After the reaction was finished, water was added and the mixture was filtered and the liquid layer was extracted with EA (20 mL x 3), the organic phase was combined and washed with water then brine, dried over Na2SC>4, concentrated and purified by prep-HPLC to get 0190-2 (2.0 g, 95.06% yield) as a white solid. Agilent LCMS 1200-6120, Column: Halo Cl 8 (30 mm*4.6 mm*2.7 pm); Column Temperature: 40 C; Flow Rate: 3.0 mL/min; Mobile Phase: from 95% [water + 10 mM TFA] and 5% [CH3CN] to 0% [water + 10 mM TFA] and 100% [CH3CN] in 0.8 min, then under this condition for 0.4 min, finally changed to 95% [water + 10 mM TFA] and 5% [CH3CN] in 0.01 min. Purity is 93.35%. Rt = 0.853 min; MS Calcd.:282.7; MS Found: 283.7 [M+H]+.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
120K+ Compounds
Competitive Price
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