HRID17781

反应详情

EQUATION

反应方程式

HRID 17781 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The ketone was prepared in the same manner as the benzotriazole aldehyde from 5-aminobenzotriazole and acetaldoxime. Column chromatography of the crude ketone using DCM and eluting with MeOH (0-10%) afforded the ketone in 11% yield. Rf [A] 0.3; δH(400 MHz; Acetone-d6) 2.68 (3H, s, CH3), 7.92 (1H, d, J 8.7, Ar—H), 8.07 (1H, d, 3 8.7 Ar—H), 8.62 (1H, s, Ar—H); m/z (FAB−HR) 162.06674 [(M+H)+ calc. for C8H8N3O 162.06682]. The hydrazone of the ketone was prepared from 2,4DNPH to afford an orange solid. 4,6-Dinitro-7-1H-benzotriazole [26]

WORKUP

后处理

  1. washeluting with MeOH (0-10%)