To a stirred suspension of lithium aluminium deuteride (1.96 g, 51.7 mmol, 3 equiv) in 25 ml of dry THF under argon was added methyl valerate (2.25 ml, 17.2 mmol, 1 equiv) in 5 ml of dry THF drop wise.
To a solution of 100 ml of 1.0 M BBr3 in dichloromethane in a dried 250 ml three necked flask was added a solution of 5.40 g of 3,5-dimethoxybromobenzene in 10 ml of dry dichloromethane over 30 minutes.
The resulting mixture was stirred at 60 °C for 1 h and [1-2H2]n-pentyl-4-methylbenzenesulfonate [1-2H2]n-pentyl-4-methylbenzenesulfonate [1-2H2]n-pentyl-4-methylbenzenesulfonate [1-2H2]n-pentyl-4-methylbenzenesulfonate [1-2H2]n-pentyl-4-methylbenzenesulfonate 29
To a stirred suspension of sodium hydride (471 mg, 19.7 mmol, 14.8 equiv) in 10 ml of dry DCM, under argon, was added distilled dimethyl malonate (2.70 g, 20.5 mmol, 5 equiv) in 15 ml dry of THF drop wise.
Three hundred (300) mg (1 mmol) of (2) was dissolved in 20 mL of dry MeOH.
Whole pouches in their glass vials were extracted with 20 mL of dry methanol with shaking (180 rpm, 30 min).
It was washed with 50 mL of dry ether in 5 aliquots when an amorphous solid was obtained.
This pasty mass was washed with little amount of hot ethanol and then with 50 mL of dry ether.
Typically, a solution of 5 mL of 33% ammonia solution was mixed with 50 mL of dry ethanol.
were added to 50 mL of dry pyridine, containing (0.015 molar eq). of aniline, to form a solution.
The aldehyde precursor (3.8 mg) dissolved in 2 mL of dry DMSO was added to the dried 18F− kryptofix complex.
