反応 #630056

ord-c472f31ab7d946b39fc16452752915a1

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the ethanol was evaporated at 40° C. under reduced pressure
  2. 2
    workup.ADDITION9.9 ml of 2N hydrochloric acid were added to the aqueous solution
  3. 3
    workup.WAITthe mixture stood at 0° to 5° C. for 16 hours
  4. 4
    ろ過was filtered
  5. 5
    その他to remove chlorides
  6. 6
    その他was dried at room temperature under reduced pressure of 0.5 to 1 mmHg

実験手順

A mixture of 4 g of the product of Example 16, 10 ml of 2N sodium hydroxide and 20 ml of ethanol was stirred at 60° C. under argon for 30 minutes and the ethanol was evaporated at 40° C. under reduced pressure. 9.9 ml of 2N hydrochloric acid were added to the aqueous solution and the mixture stood at 0° to 5° C. for 16 hours and was filtered. The recovered product was empasted several times with ice water to remove chlorides and was dried at room temperature under reduced pressure of 0.5 to 1 mmHg to obtain 3.6 g of 5-(4-methoxyphenyl)-4-phenyl-4H-1,2,4-triazole-3-acetic acid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04659729uspto-grants-1987_04