Amidines was warmed on a steam bath for 2 hr. The volatiles were removed under reduced pressure and the residue was taken up in 5% aqueous HCI and washed with Et20. Excess K2C03 was added and the product extracted (Et20), dried (Na2S04), and treated with Et20-HCI. The salt was recrystallized twice from Me,CO to afford 4.3 g (73%) of product: mp 160-161°; ir (KBr) 1770 (ester 0=0); nmr (D,0) 2.40 (s 6, CH3COOAr), 2.95 (s, 6, N(CH3)2), 3.25 (m, 4, CHjCHj), 7.30 (m, 3, Ar H). Anal. (C14H20NO4Cl) C, , N.
Bis‐(p‐nitrophenyl)‐sulfon (I) wird in 80%igem Äthanol in Gegenwart geringe Mengen Essigsäure mit Zinkstaub und Ammoniumchlorid zu dem Bis‐hydroxylamin‐Derivat (II) reduziert, das mit Essigsäureanhydrid unter Erwärmen z 4,4′‐Bis‐(N,O‐diacetylhydroxylamino)‐diphenylsulfon (III) umgesetzt werden kann.
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