反应 #5041

ord-05c3ddf43a57421683e130c85cd4575d

反应方程式

CI
methyl iodide
c1ccc(COc2ccc(-c3nnn[nH]3)cc2)cc1
tetrazole
c1ccc(COc2ccc(-c3nnn[nH]3)cc2)cc1
5-(4-benzyloxyphenyl)tetrazole
CCN(C(C)C)C(C)C
DIPEA
Cn1nnc(-c2ccc(OCc3ccccc3)cc2)n1
2-methyl-5-(4-benzyloxyphenyl)-2H-tetrazole

反应条件

温度
18°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05242924uspto-grants-1993_09