Dimethyl-2-nitroterephthalat

Bezeichnung:Dimethyl-2-nitroterephthalat

CAS-Nr5292-45-5

Englisch Name:Dimethyl nitroterephthalate

CBNumberCB9728811

SummenformelC10H9NO6

Molgewicht239.18

MOL-Datei5292-45-5.mol

Synonyma

Dimethyl-2-nitroterephthalat

Dimethyl-2-nitroterephthalat physikalisch-chemischer Eigenschaften

Schmelzpunkt	73-76 °C(lit.)
Siedepunkt	381.83°C (rough estimate)
Dichte	1.272
Dampfdruck	0.014Pa at 20℃
Brechungsindex	1.5310 (estimate)
storage temp.	Sealed in dry,Room Temperature
Aggregatzustand	Powder
Farbe	White to Almost white
Wasserlöslichkeit	INSOLUBLE
BRN	1993064
LogP	1.78 at 23℃ and pH3.6
CAS Datenbank	5292-45-5(CAS DataBase Reference)
EPA chemische Informationen	1,4-Benzenedicarboxylic acid, 2-nitro-, dimethyl ester (5292-45-5)

Sicherheit

Kennzeichnung gefährlicher	Xi
R-Sätze:	36/37/38
S-Sätze:	37/39-26-24/25
WGK Germany	2
TSCA	TSCA listed
HS Code	29173990

Gefahreninformationscode (GHS)

Dimethyl nitroterephthalate Chemische Eigenschaften,Einsatz,Produktion Methoden

R-Sätze Betriebsanweisung:
R36/37/38:Reizt die Augen, die Atmungsorgane und die Haut.
S-Sätze Betriebsanweisung:
S37/39:Bei der Arbeit geeignete Schutzhandschuhe und Schutzbrille/Gesichtsschutz tragen.
S26:Bei Berührung mit den Augen sofort gründlich mit Wasser abspülen und Arzt konsultieren.
Chemische Eigenschaften
white powder
Synthese

120-61-6

5292-45-5

In a 1000 ml four-necked flask, 926.97 g of 98% concentrated sulfuric acid was added with stirring and the temperature was maintained at 10 to 15°C. 200.72 g of 97.7% nitric acid was added slowly and dropwise. After the nitric acid was added, 300.0 g of dimethyl terephthalate was added and the reaction temperature was maintained at 10 to 15°C for about 30 minutes. Subsequently, the reaction temperature was controlled at 15 to 20°C and the reaction was continued for 30 minutes before the endpoint of the reaction was monitored by thin layer chromatography (TLC). Upon completion of the reaction, the reaction mixture was stirred for 15 minutes, filtered, and the filter cake was sequentially washed to neutrality with 900 mL of 5% aqueous sodium hydroxide and 500 mL of water. The filter cake was suspended in 3000 ml of water and stirred for 30 min at room temperature. Next, the mixture is transferred to a recrystallization unit and 1500 g of ethanol is added for recrystallization: the solid is first heated to 50 to 55°C to dissolve completely, then slowly cooled to below 5°C to promote full precipitation of the product. The precipitate was collected by filtration and dried to give 382.5 g of crude product. Further vacuum drying at 60°C gave 351.2 g of the white crystalline product, dimethyl 2-nitroterephthalate, in 95% yield (as dimethyl terephthalate). The product was analyzed by gas chromatography and showed a purity of greater than 99% with a melting point of 73.8 to 75.5°C (literature value: 73 to 76°C).
Einzelnachweise
[1] Journal of Organic Chemistry, 2001, vol. 66, # 12, p. 4356 - 4360
[2] Patent: CN103524386, 2016, B. Location in patent: Paragraph 0029; 0030; 0031
[3] Patent: CN104072403, 2016, B. Location in patent: Paragraph 0031-0033
[4] Liebigs Annalen der Chemie, 1987, p. 833 - 838
[5] Justus Liebigs Annalen der Chemie, 1912, vol. 393, p. 25

Dimethyl nitroterephthalate Upstream-Materialien And Downstream Produkte

Dimethyl-2-nitroterephthalat Anbieter Lieferant Produzent Hersteller Vertrieb Händler.

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