Chemistry of carbon compounds – Miscellaneous organic carbon compounds – C-metal
Patent
1975-05-27
1977-10-04
Jiles, Henry R.
Chemistry of carbon compounds
Miscellaneous organic carbon compounds
C-metal
C07D30771
Patent
active
040524191
ABSTRACT:
A method of preparing 5-nitrofurfural diacetate which comprises nitration furfural or furfural diacetate at a temperature within the range of from -10.degree. to +10.degree. C; said nitration being effected by the gradual simultaneous addition of furfural or a furfural diacetate solution in acetic anhydride and a mixture of nitric and sulphuric acids into acetic anhydride at a temperature within the range of from -10.degree. to +10.degree. C under continuous stirring of the reaction mixture. In doing so, molar proportions of furfural or furfural diacetate and nitric acid and sulphuric acid are maintained equal to 1:1.1-2:0.036-0.041 respectively and said compounds are added into acetic anhydride at such rates as to maintain the nitration reaction temperature at a predetermined level. The reaction mixture resulting from the nitration is treated with water at a weight ratio between water and the starting acetic anhydride ranging from 1.1:1 to 1.8:1 respectively and at a temperature within the range of from 0.degree. to 15.degree. C; the reaction mixture is then neutralized with an alkali to a pH = 3.5 - 5 at a temperature within the range of from 0.degree. to 25.degree. C, maintained at a temperature of from 45.degree. to 55.degree. C, and the desired product is thereafter isolated from said reaction mixture.
REFERENCES:
patent: 2490006 (1949-11-01), Kimel et al.
Wagner et al., Synthetic Organic Chem., New York, John Wiley Inc., (1959), pp. 746-748.
Berggrin Guntis Erikovich
Brinkmanis Robert Avgustovich
Giller Solomon Aronovich
Mikstais Uldis Yanovich
Stankevich Paul Alexandrovich
Dentz Bernard
Jiles Henry R.
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