* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Reference：
[1] Industrial and Engineering Chemistry, 1955, vol. 47, p. 358,359
[2] Revue de Chimie, Academie de la Republique Populaire Roumaine, 1956, vol. 1, # 1, p. 155,163
[3] Journal of the American Chemical Society, 1950, vol. 72, p. 756
2
[ 92-55-7 ]
[ 4426-72-6 ]
[ 59-87-0 ]
Reference：
[1] Industrial and Engineering Chemistry, 1955, vol. 47, p. 358,359
[2] Revue de Chimie, Academie de la Republique Populaire Roumaine, 1956, vol. 1, # 1, p. 155,163
[3] Journal of the American Chemical Society, 1950, vol. 72, p. 756
3
[ 92-55-7 ]
[ 110-20-3 ]
[ 59-87-0 ]
Reference：
[1] Patent: US2866795, 1956, ,
4
[ 92-55-7 ]
[ 698-63-5 ]
Yield
Reaction Conditions
Operation in experiment
89.2%
at 78 - 85℃; for 1.5 h;
100 l) was charged with 60 L of ethanol, 50 kg of 5-nitro-furfural (compound l), 20 kg (82.25 mol), and 10percent of sulfuric acid (^ (3) (4.11111, 111):Heated to 78 to 85 ° C, reacted for 1 and 5 h, concentrated under reduced pressure to remove ethanol to give a concentrate; the concentrate was dissolved in methylene chloride and washed three times with saturated sodium chloride to collect the methylene chloride layer; The crude product was purified by silica gel column chromatography (eluent PE: EA = 5: 1). The crude product was collected and the residue was purified by solidification on silica gel. Concentrated to give 5 - nitro - furfural pure product, the yield was 89.2percent.[0077] If the preparation of nitramine too Seoul, then the reaction of the product without purification separation, directly used for the preparation of Nasisi Taier.[0078] (2) Preparation of nitrofurant crude[0079] In the dark conditions, 3-amino-5-methylthiomethyl-2-oxazolidinone (compound3) 14. 7 kg (90.66 mil) in ethanol (20 L) was added to the reaction solution (60 L) of step (1) cooled to 15 to 25 ° C of 5-nitro-furfural (compound 2) After precipitation, the reaction was carried out at 20 to 25 ° C for 2 hours. The solid was filtered and the residue was filtered. The filter cake was washed with cold ethanol (5 to 10 ° C) and dried to obtain crude nitrofurant.(3) refinement of nitrofurant[0081] in the dark conditions, take nitrofurant crude 5kg, add 95percent ethanol 60L, heated to reflux, hot filter to get the filtrate; the filtrate to stand, precipitate solid, filter, filter cake with a small amount of 95percent ethanol , The solvent was removed and dried to constant weight to give a light yellow nitrofurant extract with a yield of 95percent and a total yield of 85.2percent.
88%
With sulfuric acid In water at 100℃; for 0.166667 h;
A mixture of 5-nitrofurfural diacetate(2) (10 g, 41.12 mmol) and 50 percent aqueous sulphuric acid (100mL) was heated to 100 °C for 10 min. After completion of the reaction, checked by TLC, the reaction mixture was cooled to room temperature and extracted with ethyl acetate (2 × 100 mL)and the organic layer was washed with water, brine solution and dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure to obtain 5-nitrofurfural 3. Yield:5.10 g, 88 percent. m.p.: 35-36 °C.
Reference：
[1] Phosphorus, Sulfur and Silicon and the Related Elements, 2004, vol. 179, # 12, p. 2645 - 2651
[2] Molecules, 2009, vol. 14, # 10, p. 4065 - 4078
[3] Patent: CN105820145, 2016, A, . Location in patent: Paragraph 0075-0081
[4] Asian Journal of Chemistry, 2018, vol. 30, # 2, p. 312 - 316
[5] Journal of Organic Chemistry, 2018, vol. 83, # 8, p. 4427 - 4440
[6] Journal of Chemical Research, Miniprint, 1989, # 6, p. 1201 - 1218
[7] Journal of the American Chemical Society, 1930, vol. 52, p. 2550,2551
[8] Journal of the Indian Chemical Society, 1981, vol. 58, p. 217 - 219
[9] Tetrahedron Letters, 1995, vol. 36, # 11, p. 1779 - 1782
[10] Collection of Czechoslovak Chemical Communications, 1996, vol. 61, # 8, p. 1233 - 1243
[11] Patent: WO2005/14585, 2005, A1, . Location in patent: Page/Page column 18
[12] Archiv der Pharmazie, 2007, vol. 340, # 12, p. 635 - 641
[13] Patent: CN103664923, 2016, B, . Location in patent: Paragraph 0049
[14] Patent: CN104402874, 2016, B, . Location in patent: Paragraph 0067; 0071; 0072; 0073
[15] Patent: CN103755696, 2016, B, . Location in patent: Paragraph 0047
[16] Patent: CN107987069, 2018, A, . Location in patent: Paragraph 0024; 0066-0071
[17] Patent: CN108084174, 2018, A, . Location in patent: Paragraph 0068; 0069; 0070; 0073
[18] Patent: CN108383834, 2018, A, . Location in patent: Paragraph 0032; 0035; 0037; 0042; 0047
5
[ 98-01-1 ]
[ 108-24-7 ]
[ 92-55-7 ]
Yield
Reaction Conditions
Operation in experiment
82%
at 0℃; for 2.41667 h;
A premixed solution of concentrated nitric acid (8.6 mL, 12.2 g, 193.62 mmol) and concentrated sulphuric acid (0.06 mL, 1.1 g, 11.2 mmol) was added drop-wise into acetic anhydride (90 mL) at 0 °C with stirring. To the above reaction mixture, furfural (1) (freshly distilled, 10.4 mL, 12.06 g, 125.5 mmol) was added drop-wise over a period of 45 min and stirred for 1 h at 0 °C. Water (100 mL) was added to the mixture and stirred at room temperature for 30 min to obtain a white precipitate. To the reaction contents, 10 percent NaOH solution was added until the pH of the mixture reached about 2.5 and the mixture was heated at 50 °C for 1 h. After cooling to room temperature, the white precipitate formed was filtered, washed with water, recrystallized from anhydrous ethanol and dried to obtain diacetate compound 2.Yield: 24.84 g, 82 percent.
Reference：
[1] Asian Journal of Chemistry, 2018, vol. 30, # 2, p. 312 - 316
[2] Journal of Organic Chemistry, 2018, vol. 83, # 8, p. 4427 - 4440
[3] Industrial and Engineering Chemistry, 1955, vol. 47, p. 358,359
[4] Kagaku Kenkyusho Hokoku, 1955, vol. 31, p. 430,434[5] Chem.Abstr., 1956, p. 15504
[6] Patent: US2502114, 1947, ,
[7] Journal of Chemical Research, Miniprint, 1989, # 6, p. 1201 - 1218
[8] Collection of Czechoslovak Chemical Communications, 1996, vol. 61, # 8, p. 1233 - 1243
[9] Indian Journal of Heterocyclic Chemistry, 2011, vol. 20, # 4, p. 313 - 316
Reference：
[1] Journal of Organic Chemistry, 1986, vol. 51, # 20, p. 3811 - 3818
[2] Journal of Organic Chemistry, 1986, vol. 51, # 20, p. 3811 - 3818
8
[ 5904-70-1 ]
[ 92-55-7 ]
Reference：
[1] Tohoku J. agric. Res., 1954, vol. 5, p. 147,148
[2] Journal of the American Chemical Society, 1930, vol. 52, p. 2550,2551
[3] Yakugaku Zasshi, 1955, vol. 75, p. 424[4] Chem.Abstr., 1956, p. 2539
[5] Yakugaku Zasshi, 1955, vol. 75, p. 424[6] Chem.Abstr., 1956, p. 2539
[7] Yakugaku Zasshi, 1955, vol. 75, p. 424[8] Chem.Abstr., 1956, p. 2539
9
[ 75631-82-2 ]
[ 92-55-7 ]
Reference：
[1] Journal of Organic Chemistry, 1986, vol. 51, # 20, p. 3811 - 3818
10
[ 6301-02-6 ]
[ 92-55-7 ]
[ 67-20-9 ]
Reference：
[1] Yakugaku Zasshi, 1955, vol. 75, p. 117,119, 120[2] Chem.Abstr., 1956, p. 1782
11
[ 109-84-2 ]
[ 92-55-7 ]
[ 67-45-8 ]
Reference：
[1] Industrial and Engineering Chemistry, 1955, vol. 47, p. 358,359
[2] Przemysl Chemiczny, 1957, vol. 36, p. 400[3] Chem.Abstr., 1958, p. 3140
12
[ 92-55-7 ]
[ 20782-91-6 ]
Reference：
[1] Asian Journal of Chemistry, 2018, vol. 30, # 2, p. 312 - 316
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