反応 #94476

ord-5e927bfc05ae4f908ad3f1fd1de1f6e2

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他prepared
  2. 2
    その他at 10° C
  3. 3
    濃縮at 25° C., the mixture is concentrated under reduced pressure
  4. 4
    workup.STIRRINGthe residual material stirred with water
  5. 5
    その他collected
  6. 6
    その他Triturating the filter cake with acetone

実験手順

4-Nitrostyrylsulfonyl chloride (2.5 g., 0.01 mole) is added portion-wise to a solution of 4-nitrobenzamidine (1.65 g., 0.01 mole), prepared according to the procedure of L. Weintraub, et al., J. Org. Chem., 33, 1679 (1968), and triethylamine (1.01 g., 0.01 mole) in 50 ml. of acetone at 10° C. After stirring for a period of 1 hr. at 25° C., the mixture is concentrated under reduced pressure and the residual material stirred with water and collected. Triturating the filter cake with acetone provides N-(4-NITROSTYRYLSULFONYL)-4-NITROBENZAMIDINE, m.p. 173°-177° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04130663uspto-grants-1978_12