Abstract
The synthesis of 6-nitro veratraldehyde from vanillin was used HNO3 and a mixture of HNO3 and H2SO4. The reaction steps were (I) methylation of vanillin and (2) nitration of the methylation product. Methylation of vanillin was conducted using dimetnylsulfate and NaOH at 60 0C for 2 hours. Nitration of the methylation product was performed in two methods, which using HN03 and using a mixture of HN03 and H2SO4 both at 5 0C for 2 hours. The products were analyzed by means of TLC, GC; IR, 1H-NMR and GC-MS spectrometers.The methylation of vanillin gave 87.7 % yield of veratraldehyde which was found as a white crystal (m.p 43 oC). The nitration of veratraldehyde produced 6-nitro veratraldehyde observed as a yellow crystal having of m.p. 1300C. Nitration using neat HNO3 gave a smaller yield (50.35%) of 6-nitro veratraldehyde than nitration with a mixture of HNO3 and H2SO4 (93.63 %).
Highlights
Nitration of the methylation product was performed in two methods, which using HN03 and using a mixture of HN03 and H2SO4 both at 5 0C for 2 hours
The methylation of vanillin gave 87.7 % yield of veratraldehyde which was found as a white crystal (m.p 43 oC)
The nitration of veratraldehyde produced 6-nitro veratraldehyde observed as a yellow crystal having of m.p. 130 0C
Summary
Alat yang digunakan adalah alatalat gelas, alat refluks, evaporator Buchi, Desikator, IR, Shimadzu - FTIR 8201 PC, 'H-NMR, JEOL - MY60, GC-MS, Shimadzu QP - 5000, Lampu UV(Camac UV - Cabinet II), GC, HP 6890 Series. Vanilin 10 g (0,065 mol) dalam 25 mL air panas dimasukkan ke dalam labu leher tiga, yang telah dilengkapi dengan pendingin balik, pengaduk magnet dan dua corong penetes. Campuran dipanaskan sampai suhu 60 oC dan ditambahkan dimetil sulfat sebanyak 9,2 mL (0,09 mol) tetes demi tetes. Penambahan larutan NaOH dan dimetil sulfat dilakukan secara bergantian lebih dari dua kali, sehingga total dimetil sulfat yang ditambahkan adalah 16,8 mL (22,4 g, 0,18 mol). Nitrat Asam nitrat (12,6 g, 0,194 mol) dimasukkan ke dalam labu leher tiga yang telah dilengkapi dengan termometer, corong penetes dan pengaduk magnet. Endapan yang terbentuk disaring dengan penyaring Buchner, dicuci dan dikeringkan dalam desikator. 2.2 Nitrasi Veratraldehid dengan Campuran Asam Nitrat dan Asam Sulfat Asam sulfat pekat (1,67 g; 0,017 mol) dimasukkan ke dalam labu leher tiga yang telah dilengkapi dengan termometer, corong penetes dan pengaduk magnet. Analisa hasil reaksi dilakukan dengan menggunakan spektrofotometer IR, 1NMR dan GC-MS
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