تفاعل #64554

ord-8e3ad536e2b044d0b3e1ff63c3a2902a

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىPurification of the crude product by flash chromatography on silica gel (gradient elution with 1-4% MeOH in CH2Cl2)

الإجراء التجريبي

By the procedure of Example 69, 2-(5-amino-2-chlorophenyl)-5-n-butyl-4-[[2'-[N-(2-chlorobenzoyl)sulfamoyl]-5'-ethylbiphenyl-4-yl]methyl]-2,4-dihydro-3H-1,2,4-triazol-3-one (from Step D) was reacted with propionyl bromide in the presence of DMAP. Purification of the crude product by flash chromatography on silica gel (gradient elution with 1-4% MeOH in CH2Cl2) afforded a 65% yield of the title compound as a cream-colored solid, mp 144°-146° C.; homogeneous by TLC in 9:1 CH2Cl2 --MeOH; m/e 734 (M+1)+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05411980uspto-grants-1995_05