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2-(4'-n-pentoxy[1,1']biphenyl-4-yl)-acetophenone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With sodium carbonate; In water; ethylene glycol;
Example 1 15.5 g of 2-chloroacetophenone, 31.3 g of 4'-n-pentoxybiphenyl-4-boronic acid, 7.5 g of sodium carbonate and a mixture of 44 mg of palladium as a 22% strength aqueous chloride solution, 1 ml of water and 720 mg of a 0.6M aqueous TPPTS solution together with 120 ml of ethylene glycol and 16 ml of water are placed under nitrogen in a reaction vessel and heated to boiling for 4 hours. After cooling to room temperature, 150 ml of water are added, the mixture is stirred vigorously for another 20 minutes and the solid which remains is filtered off. Crystallization of the residue from acetone and drying at 50 C. under reduced pressure gives 32 g (89%) of 2-(4'-n-pentoxy[1,1']biphenyl-4-yl)-acetophenone having a melting point of 86 C.
With hydrogenchloride; tin(ll) chloride; In aq. phosphate buffer; water; at 100℃; for 0.5h;pH 7.4;
The labeling method was as follows: to a 10 mL vial was added <strong>[5704-04-1]tricin</strong>e solution (0.5 mL, 80 mg/mLin saline), HYNIC-D1-FA2 solution (100 L, 1 mg/mL in PBS, pH 7.4), TPPTS (0.2 mL, 5 mg/mL insaline), SnCl2 solution (20 L, 2 mg/mL) in 0.1 N HCl and about 1 mL of 99mTcO4 (370 MBq) in saline.The vial was heated at 100 C for 30 min in a heating module. After cooling to room temperature,a sample of the resulting solution was purified and analyzed by Sep-Pak C18 cartridge and radio-HPLC.In further experiments, a kit formulation was developed for preparation of 99mTc-HYNIC-D1-FA2 usingthis ternary ligand system.
((6S,7R,10S)-N<SUP>10</SUP>-((S)-5-guanidino-1-((2-(6-hydrazinylnicotinamido)ethyl)amino)-1-oxopentan-2-yl)-N<SUP>6</SUP>-hydroxy-7-isobutyl-8-oxo-2-oxa-9-aza-1(1,4)-benzenacycloundecaphane-6,10-dicarboxamide)[ No CAS ]
[ 63995-70-0 ]
C58H73N12O21PS3(99)Tc(1+)[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
at 95℃; for 0.166667h;
1 was labeled with99mTc by heating99mTc in a vehicle solution containing <strong>[5704-04-1]tricin</strong>e and 3,3',3"-phosphanetriyltris(benzenesulfonic acid) trisodium salt (TPPTS) in high purity and yield. Typically, 2 mug of 1 was mixed 5-10 mCi / 100 mu99iotaetaTau04, followed by addition of with 200 of the vehicle solution in a vial. The mixture was heated at 95 C for 10 min, and cooled to room temperature to yield the99mTc-labeled product as analyzed by radio- HPLC. Radio-HPLC analysis was performed using Waters RP-HPLC (Milford, MA) on a reverse-phase analytical column (Phenomenex, Jupiter 4 mu Proteo 90A, 250 x 4.6 mm, 4 micron) with a gradient from 10% to 70 % aqueous acetonitrile containing 25 mM ammonium formate at a flow rate of 1 mL/min over 40 min.
With tin(II) chloride dihdyrate; In aq. acetate buffer; for 0.5h;pH 5;Heating;
Weigh 0.3 mg of HYNICNM ligand into a 10 mL penicillin vial. Add 0.5 mL of pH 5 sodium acetate buffer to dissolve. Then add 5mg TPPTS in turn, 5mg <strong>[5704-04-1]tricin</strong>e, 40mug SnCl 2 ·2H 2 O, Add 2 mL of freshly rinsed Na99mTcO 4 solution. The 99mTc (HYNICNM) (<strong>[5704-04-1]tricin</strong>e/TPPTS) complex was obtained by heating in a boiling water bath for 30 min.
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