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tetrakis (triphenylphosphine) palladium (O)[ No CAS ]
[ 64-02-8 ]
[ 108857-18-7 ]
[ 108857-09-6 ]
Yield
Reaction Conditions
Operation in experiment
Zinc chloride; In tetrahydrofuran; hexane; water;
EXAMPLE 4 7-(<strong>[6086-21-1]1-Methyl-1,2,4-triazol</strong>-5-yl)-1,2,3,5-tetrahydroimidazo(2,1-b)-quinazolin-2-(1H)-one, H2 O STR13 n-Butyl lithium (6.6 cm3 of a 1.6M solution in n-hexane) was added to a stirred solution of 1-methyl-1,2,4-triazole (0.83 g) in THF (20 cm3) at -70° under nitrogen. After stirring for 1 hour at -70° the white syspension was treated with a solution of anhydrous zinc chloride (4.1 g) in THF (20 cm3) and the mixture was warmed to room temperatue. 7-Iodo-1,2,3,5-tetrahydroimidazo(2,1-b)quinazolin-2-(1H)-one (1.33 g) and tetrakis (triphenylphosphine)palladium (O) (0.05 g) were added and the mixture was heated under reflux for 6 hours. The cooled solution was evaporated in vacuo and the residue partitioned between dichloromethane:methanol, 9:1 (200 cm3), and a solution of ethylenediaminetetraacetic acid disodium salt (10 g) in water (200 cm3). The aqueous phase was further extracted with dichloromethane:methanol, 9:1 (2*150 cm3), and the combined and dried (MgSO4) organic phases were evaporated in vacuo to give a solid which was chromatographed on silica (Merck "MK 60.9385" [Trade Mark]) eluding with chloroform:methanol:aqueous ammonia (S.G. 0.880), 90:10:1. Combination and evaporation of appropriate fractions afforded a solid (0.36 g) which was recrystallized from chloroform-methanol to give the title compound, m.p. 340°-343° (0.16 g). Analysis percent: Found: C,54.7; H,4.3; N,28.9; Calculated for C13 H12 N6 O.H2 O: C,54.5; H,4.9; N,29.4.
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