反応 #2825

ord-5a1f4fa16f264e7fb02a9d9377895d83

反応方程式

O=C(c1ccc([N+](=O)[O-])c(OCc2ccc(-c3ccccc3-c3nnnn3C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2)c1)N1CCOCC1
compound ( [3]-(33)-587 )
O=C(c1ccc([N+](=O)[O-])c(OCc2ccc(-c3ccccc3-c3nnnn3C(c3ccccc3)(c3ccccc3)c3ccccc3)cc2)c1)N1CCOCC1
3-[[2'-(1-triphenylmethyltetrazol-5-yl)biphenyl-4-yl]methyloxy]-4-nitrobenzoic acid morpholide
CCO
ethanol
NN.O
hydrazine monohydrate
Nc1ccc(C(=O)N2CCOCC2)cc1OCc1ccc(-c2ccccc2-c2nnnn2C(c2ccccc2)(c2ccccc2)c2ccccc2)cc1
foam
収率 116.5%
Nc1ccc(C(=O)N2CCOCC2)cc1OCc1ccc(-c2ccccc2-c2nnnn2C(c2ccccc2)(c2ccccc2)c2ccccc2)cc1
3-[[2'-(1-triphenylmethyltetrazol-5-yl)biphenyl-4-yl]methyloxy]-4-aminobenzoic acid morpholide
収率 116.5%

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The insolubles were filtered through celite
  2. 2
    濃縮the filtrate was concentrated

実験手順

A solution of the compound ([3]-(33)-587) (0.60 g) prepared in Example 37, ethanol (150 ml), and ethyl acetate (40 ml) was stirred at 70° C. for 15 minutes. After 10% Pd/C (0.10 g) and hydrazine monohydrate (1 ml) were added to the solution, the mixture was stirred at 70° C. for 1 hour. The insolubles were filtered through celite, and the filtrate was concentrated to obtain colorless foam (0.67 g). The product was purified by silica gel column chromatography (Kieselgel 60=80 g, chloroform/ethyl acetate=13/7) to obtain the compound ([3]-(34)-587) (0.09 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05731310uspto-grants-1998_03