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ChemicalBook CAS DataBase List N-N-BUTYL-4-NITRO-PHTHALIMIDE
54395-37-8

N-N-BUTYL-4-NITRO-PHTHALIMIDE synthesis

6synthesis methods
-

Yield:54395-37-8 95%

Reaction Conditions:

with sulfuric acid;HNO3 at 80; for 0.0666667 h;Temperature;

Steps:

3; 8 Example 3

(1) Refer to Figure 3 to determine the microchannel reactor connection mode. The channel type is cylindrical straight channel and triangular microchannel structure. The number of microchannel mixed reaction modules is determined according to the flow rate and residence time, and the heat exchange medium is heat transfer oil.The N-n-butylphthalimide-concentrated sulfuric acid solution was regarded as the raw material A, the concentrated nitric acid solution was regarded as the raw material B, and the two materials were injected into the reactor through the metering pump at flow rates of 15 ml/min and 35 ml/min, respectively. In the thermal module, after the two materials are fully preheated separately, they enter the reaction zone for mixing reaction. At this time, the molar ratio of concentrated nitric acid to substrate is controlled to be 1.3:1, and the mass ratio of substrate to concentrated sulfuric acid is 1:4. The microchannel reactor of Fig. 2 was used to control the temperature at 80 ° C and the residence time was 240 s. The reaction solution was quantitatively collected, washed in an ice water bath, washed with water, filtered and dried to obtain N-n-butyl-4-nitrophthalimide. Nitrification product, HPLC content analysis (normalized) 95%, yield 95%.

References:

CN109305933,2019,A Location in patent:Paragraph 0052; 0053; 0054; 0067; 0068; 0069

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