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ChemicalBook CAS DataBase List 2-CHLORO-1,3-DIFLUORO-5-NITRO-BENZENE
3828-41-9

2-CHLORO-1,3-DIFLUORO-5-NITRO-BENZENE synthesis

4synthesis methods
-

Yield:3828-41-9 90%

Reaction Conditions:

with formamide in N,N-dimethyl-formamide at 60;Reagent/catalyst;Solvent;

Steps:

11 Example 11

50 g of 2,4-difluoro-3-chloronitroaniline was dissolved in 300 g of N, N-dimethylformamide,spare.74 g of t-butyl nitrite (mol of t-butyl nitrite: 2,4-difluoro-3-chloronitroaniline = 3: 1) was added to a 1000 ml dark-300 g of N, N-dimethylformamide,Heating up to 60 ,The above-mentioned standby solution was started to drop.Drip added insulation to complete reaction,Distillation under reduced pressure to get 3,5-difluoro-4-chloronitrobenzene crude,And then decompressed in addition to high-purity 3,5-difluoro-4-chloronitrobenzene (purity 99%, yield 60%).; On the basis of Example 1,To the initial 1000ml dark four bottles were added 4.9g cuprous chloride (mol than chlorinatedCuprous: 2,4-difluoro-3-chloronitroaniline = 0.25: 1),Other conditions remain unchanged,High purity 3,5-difluoro-4-chloronitrobenzene (purity 99%, yield 69%).; To the beginning of 1000ml dark four bottles of additives added 40g urea (mol than urea:2,4-difluoro-3-chloronitroaniline = 3: 1),Other conditions remain unchanged,High purity 3,5-difluoro-4-chloronitrobenzene (purity 99%, yield 78%).; On the basis of Example 3,Using different solvents instead,The low boiling solvent is recovered by atmospheric distillation,Other conditions remain unchanged.The results obtained are shown in Table 1; On the basis of Example 8,Using different additives (mol ratio unchanged) instead,The low boiling solvent is recovered by atmospheric distillation,Other conditions remain unchanged.The results obtained are shown in Table 2.

References:

CN106117067,2016,A Location in patent:Paragraph 0019; 0020; 0021; 0022; 0023; 0024; 0025-0032

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