Organic Chemistry of Explosives

(coco) #1
Oxidation of arylamines, arylhydroxylamines and other derivatives 153

Table 4.2 Oxidation of arylamines with peroxycarboxylic acids


NH 2

NO 2

NH 2
O 2 N NO 2

NO 2
NH 2
CH 3 CO 3 H

OCH 3

NH 2
SO 3 H

NH 2
CH 3

NH 2

NH 2

NH 2
NO 2

CF 3 CO 3 H

NO 2

NO 2

NO 2
O 2 N NO 2

NO 2
NO 2

OCH 3

NO 2
SO 3 Na

NO 2
CH 3

NO 2

NO 2

NO 2
NO 2

Entry Substrate Conditions Product Yield (%)

25163

82164

maleic anhydride,
90 % H 2 O 2 , CH 2 Cl 2
(HO 2 C-CH=CH-CO 3 H)

87166

74165

CHCl 3 , H 2 SO 4 (cat),
Ac 2 O, 90 % H 2 O 2 , reflux

1

2

4

3

5a

5b

6a

6b

7 92168

90 % H 2 O 2 , (CF 3 CO) 2 O,
CH 2 Cl 2 , reflux^86

167

89167

92167

81167

(66)

(68)

(72)

(70)

(74)

(76)

(78)

(67)

(69)

(73)

(71)

(75)

(77)

(79)

90 % H 2 O 2 , CF 3 CO 2 H,
CH 2 Cl 2 , reflux

90 % H 2 O 2 , (CF 3 CO) 2 O,
CH 2 Cl 2 , reflux

90 % H 2 O 2 , CF 3 CO 2 H,
CH 2 Cl 2 , reflux


  1. 30 % H 2 O 2 , CH 3 CO 2 H
    70–75 °C

  2. NaHCO 3


These solutions readily oxidize nitroanilines to the corresponding dinitrobenzenes but are


unable to oxidize amines of lower basicity like the dinitroanilines.^163 ,^164 Peroxyacetic acid


is well suited for the oxidation of arylamines containing strong electron-donating groups


(Table 4.2, Entry 2). Stronger oxidants like peroxytrifluoroacetic acid rapidly degrade such


substrates and give rise to various phenolic by-products. Peroxyacetic acid is also the reagent


of choice for the oxidation of some condensed ring arylamines (Table 4.2, Entry 1).^163


The reagent prepared from the reaction of 30 % hydrogen peroxide with glacial acetic acid


also contains peroxyacetic acid but the main product of arylamine oxidation is usually the


corresponding nitroso compound.^169 ,^170 On heating with an excess of this reagent the nitro


compound is usually obtained.^165 ,^169

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