2,3-Difluorobenzaldehyde synthesis

Yield:2646-91-5 48.2%

Reaction Conditions:

with sodium molybdate;dihydrogen peroxide;cobalt(II) acetate;acetic acid;sodium bromide at 120;Temperature;

Steps:

9
(1) Apparatus: The connection type of the tubular reactor is determined according to Fig. 2, and the pipe type is: (3a + 3c) DC type channel + inclined square cake type variable diameter flat pipe,Pipeline diameter and volume according to the flow rate and reaction time to determine,Heat transfer medium for the heat transfer oil.(2) 6.06 g of cobalt acetate and 6.06 g of sodium molybdate were respectively dissolved200 mg of 2,3-difluorotoluene and 200 ml of acetic acid to form a mixed solution at which time n (cobalt acetate): n (2,3-difluorotoluene) = 0.015: 1, 6.06 g of sodium bromide was dissolved in35% H2O2 to form H2O2-acetic acid solution, then n (sodium bromide):N (2,3-difluorotoluene) = 0.015: 1,2,3-difluorotoluene-acetic acid solution with andH2O2-acetic acid solution at 5.56 ml / min and 11.11 ml / min, respectivelyOf the flow rate through the constant current pump into the continuous heat exchanger tube reactor,At this time n (H2O2): n (2,3-difluorotoluene) = 2: 1, using Figure 2 microchannel reactor,Control reaction temperature 120 , residence time 1500s. Export material 0 cooling,The reaction was quenched with difluoromethane. After GC analysis,The conversion of 2,3-difluorotoluene was 65.1% and the yield of 2,3-difluorobenzaldehyde was 48.2%.

References:

Changzhou University;Liu Jianwu;Jiang Xin;Zhang Yue;Yan Shenghu;Shen Jiefa;Ma Xiaoming;Chen Daixiang;Gu Shunlin;Ni Fengchao;Li Yanfei;Wang Qiuhong;Chen Mingzhu CN106748682, 2017, A Location in patent:Paragraph 0052-0054

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