تفاعل #487500

معادلة التفاعل

methyl magnesium bromide

1,2-bis(diphenylphosphino)ethane

phenylazide

THF

→

Acetoanilide

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas pre-charged with [11C]CO
2. 2
   أخرىwas flushed with N2 (the [11C]CO-
3. 3
   workup.DISSOLUTIONThe solution was dissolved in ammonium formate (0.5 mL, pH=3.5)
4. 4
   درجة الحرارةheated at 120° C. for 1 min
5. 5
   أخرىA small amount of crude product was collected

الإجراء التجريبي

In a capped vial (1 mL) containing a solution of phenylazide (6.6 mg, 55 μmol) in dry THF (300 μL), was added [RhCl(cod)]2 (0.27 mg, 0.55 μmol), and 1,2-bis(diphenylphosphino)ethane (0.66 mg, 1.65 μmol), and was shaken until the solution was homogeneous. After addition of a solution of methyl magnesium bromide (18.5 μL of 3M solution in ether, 55 μmol), the resulting mixture was transferred to the micro-autoclave, which was pre-charged with [11C]CO. The micro-autoclave was heated at 120° C. for 5 min under 35 MPa and the crude product was transferred to a reduced pressure vial. The radioactivity was measured before and after the vial was flushed with N2 (the [11C]CO-trapping efficiency of 96% was determined based on these values). The solution was dissolved in ammonium formate (0.5 mL, pH=3.5) and heated at 120° C. for 1 min. A small amount of crude product was collected and analyzed by the reversed phase HPLC. Yield of product: 91%. The product was identified by HPLC with an added authentic reference compound.

المصدر