Reaktion #5041

Reaktionsgleichung

methyl iodide

tetrazole

5-(4-benzyloxyphenyl)tetrazole

DIPEA

→

2-methyl-5-(4-benzyloxyphenyl)-2H-tetrazole

Lösungsmittel

NMP

NMP

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to 18° C
2. 2
   SonstigeThe resulting solid was collected
3. 3
   Waschenwashed with water
4. 4
   Sonstigerecrystallized from ethanol
5. 5
   Sonstigedried in vacuo at 50° C.

Vorschrift

To a stirred solution containing 337 g of the tetrazole and 362 mL of DIPEA in 1 L of NMP cooled to 18° C. under N2 was added dropwise over 1.5 hrs 200 g of methyl iodide in 170 mL NMP. After stirring an additional hour at room temperature, the reaction mixture was diluted with 340 mL of water and the reaction mixture was diluted with 340 mL of water and cooled to 18° C. The resulting solid was collected, washed with water, recrystallized from ethanol and dried in vacuo at 50° C. to give 232.3 g of 2-methyl-5-(4-benzyloxyphenyl)-2H-tetrazole.

Quelle