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ChemicalBook CAS DataBase List 4,5-DICHLOROPHTHALIC ANHYDRIDE

4,5-DICHLOROPHTHALIC ANHYDRIDE synthesis

4synthesis methods
-

Yield:942-06-3 100%

Reaction Conditions:

with acetyl chloride for 2 h;Reflux;

Steps:

5.1.19 5,6-Dichlorophthalic anhydride (40)
Diacid 39 (10.00 g, 42.55 mmol) was suspended in AcCl (50 mL) and the mixture was heated at reflux with stirring for 2 h.
The obtained suspension was concentrated in vacuo and azeotroped with hexanes (2 * 10 mL) and PhMe (2 * 10 mL) to provide anhydride 40 (9.23 g, 100%) as a beige powder, Rf (SiO2, CHCl3) 0.64: mp 185-189 °C. 1H NMR (500 MHz, CDCl3) δ 8.10 (s, 2H); CIMS m/z (rel intensity) 217/219/221 (MH+, 100/69/12).

References:

Beck, Daniel E.;Lv, Wei;Abdelmalak, Monica;Plescia, Caroline B.;Agama, Keli;Marchand, Christophe;Pommier, Yves;Cushman, Mark [Bioorganic and Medicinal Chemistry,2016,vol. 24,# 7,p. 1469 - 1479]

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