반응 #5041

반응 방정식

methyl iodide

tetrazole

5-(4-benzyloxyphenyl)tetrazole

DIPEA

→

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

용매

NMP

NMP

water

water

반응 조건

후처리

1. 1
   온도cooled to 18° C
2. 2
   기타The resulting solid was collected
3. 3
   세척washed with water
4. 4
   기타recrystallized from ethanol
5. 5
   기타dried in vacuo at 50° C.

실험 절차

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.

출처