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ChemicalBook CAS DataBase List 2,4,6-TRINITROBENZALDEHYDE
606-34-8

2,4,6-TRINITROBENZALDEHYDE synthesis

6synthesis methods
-

Yield:606-34-8 97.8%

Reaction Conditions:

with ozone in dichloromethane;

Steps:

6 (2) Preparation of o-nitrobenzaldehyde:

General procedure: On the microchannel reactor for gas-liquid reaction, reduce the working temperature to -10 ° C and stabilize for 10 minutes,First turn on the ozone generator to allow ozone to pass into the micro channel, so that the concentration of ozone is 10g / liter,Adjust the back pressure valve to stabilize the speed and pressure of a constant concentration of ozone gas into the microchannel,Then, 25 g of dichloromethane solution of 1,2-bis (o-nitrophenyl) ethylene obtained in step (1) was pumped through the check valve through a constant flow pump,The molar ratio of ozone to 1,2-bis (o-nitrophenyl) ethylene is 1.5: 1, and the pumping speed is controlled to achieve the optimal oxidation effect.At the outlet of the microchannel, the tail gas is collected by a gas-liquid separator to be absorbed, and the reaction liquid is collected and evaporated to recover methylene chloride to dryness.Add ethyl acetate to recrystallize, filter and wash with 0-5 ethyl acetate,Then, it was dried under the condition of a vacuum of -0.07 MPa and a temperature of 40 ° C to obtain 27 g of o-nitrobenzaldehyde with a yield of 96.4%.

References:

CN110713442,2020,A Location in patent:Paragraph 0033; 0044; 0045