反応 #5041

反応方程式

methyl iodide

tetrazole

5-(4-benzyloxyphenyl)tetrazole

DIPEA

→

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

溶媒

NMP

NMP

water

water

反応条件

後処理

1. 1
   温度cooled to 18° C
2. 2
   その他The resulting solid was collected
3. 3
   洗浄washed with water
4. 4
   その他recrystallized from ethanol
5. 5
   その他dried in vacuo at 50° C.

実験手順

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.

出典