Organic Chemistry of Explosives

(coco) #1
5-Membered rings – 2N 305

7-amino-4,6-dinitrobenzofuroxan (77) (ADNBF) is more impact insensitive than 4,6-


dinitrobenzofuroxan. ADNBF (77) has been prepared^48 from the nitration ofm-nitroaniline


(75), followed by reaction of the product, 2,3,4,6-tetranitroaniline (76), with sodium azide in


acetic acid; the latter reagent resulting in displacement of the labilem-nitro group of (76)


and spontaneousin situcyclization of the resultingo-nitroarylazide. ADNBF has also been


synthesized from the nitration of 6-chlorobenzofuroxan, followed by reaction with ammo-


nia in methylene chloride.^48 A more unusual route to ADNBF involves the reaction of 4,6-


dinitrobenzofuroxan (DNBF) with a source ofN-formyl anion and oxidation of the resulting


Meisenheimer complex with nitric acid.^49 ADNBF has excellent overall properties (calculated


VOD∼7900 m/s,d= 1 .90 g/cm^3 and m.p. 270◦C) and is under advanced development in


the US.


Cl

NO 2
Cl
78

Cl
79

O 2 N

Cl N 3

O 2 N NO 2

Cl

Cl
80

N 3

NO 2

NO 2

O 2 N

Cl

N
O

NO 2

Cl
81

O 2 N

N Cl
O

NO 2

NH 2

H 2 N

N O 2 N

O

N

NO 2

N
O O

N
O

N
O

HR

O K

+

83, R = NHOH

82
(DADNBF)

NaN 3 , DMF 100 % HNO 3

PhCH 3
heat

PhCH 3 , NH 3


  1. NH 2 OH.HCl,
    KOH (aq)

  2. H+


Figure 7.31

5,7-Diamino-4,6-dinitrobenzofuroxan (DADNBF) (82), an impact insensitive high perfor-


mance explosive (VOD∼8050 m/s,d= 1 .91 g/cm^3 ), has been prepared in four steps from


1,3,5-trichloro-2,4-dinitrobenzene (78),^50 and also by treating the Meisenheimer complex


(83)^51 with excess hydroxylamine hydrochloride in aqueous base. DADNBF has also been


synthesized in five steps starting from 2-nitroaniline.^51


2 N NH 2 O 2 NH NO 2

Cl

Cl
NO 2
85

H
N

H
N

NO 2

NO 2

NO 2

O 2 N

O 2 N

Cl O 2 N Cl

H
N

H
N

Cl Cl
H
N

H
N

NO 2

NO 2

NO 2

NO 2

NO 2
NO 2

NO 2

NO 2

O 2 N NO 2

O 2 N

O 2 N

O 2 N

O 2 N

O 2 N
O 2 N

N

O
N N

O
N

NaHCO 3
+

86

87


  1. NaN 3

  2. heat, -N 2


88

84

100 % HNO 3 ,
H 2 SO 4

2

OO

Figure 7.32
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