* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With sulfur; iodine In acetone at 120 - 170℃; for 0.416667 h; Reflux
The mass ratio of 1.2: 1 aniline and m-acetylphenol was placed in a reaction vessel and heated to make diWere dissolved. Then add the mass of 0.025 trifluoromethanesulfonic acid (m-acetylphenol mass of 1 dollars), so that the threeStir well, the temperature to 190 , so that dehydration reaction. In the course of the reaction, the separation of the productionRaw water. The reaction was terminated after 6 h. The excess aniline was distilled off under reduced pressure. Steam, dark red solid that isIs 3-acetyl diphenylamine, and this compound A is named.The above-mentioned compound A was placed in a reaction vessel, and the amount of the substance was 2.3 Sulfur (compound of the compound AThe amount of 1 dollars), the volume of 250ml of acetone (sulfur and simple substance to the total mass of 1mol dollars), temperatureSo that it dissolves into a transparent liquid. Further, 0.0125 of iodine (the amount of the substance A of the compound A was 1)To 170 ° C, and the mixture was allowed to react under stirring and refluxing. After the reaction for 25 min, the reaction was terminatedAfter the basic conversion of raw materials to complete, stop stirring, gradually cooling to 120 , visible under heat conditionsYellow and black layers. Carefully pour out the upper yellow liquid, room temperature cooling precipitation yellow solid. The crude product was mixed with ethanol-waterSolvent recrystallization after the precipitation of light yellow solid, namely 2 - acetyl phenothiazine. The overall yield in this example was 90.5percentThe purity was 99.7percent by HPLC.
Reference：
[1] Patent: CN105461655, 2016, A, . Location in patent: Paragraph 0033
[2] Patent: CN105481793, 2016, A, . Location in patent: Paragraph 0038; 0041
2
[ 62-53-3 ]
[ 23699-65-2 ]
Yield
Reaction Conditions
Operation in experiment
90%
With potassium carbonate In water at 20℃;
General procedure: In a typical example, phenylboronic acid 1 (1.22 g, 1 mmol) was charged in the flask containing K2CO3 (2 equiv) in water as solvent (2 mL). To this was added aniline 2 (0.93 g, 1 mmol) and Cu–Mn catalyst, and the reaction mixture was allowed to stir at room temperature. The completion of the reaction was monitored by TLC. After completion, the base was neutralized using 2 N HCl and the catalyst was filtered off, thorough washings of water were given, extracted with ethyl acetate, and the organic layer was separated and dried under reduced vacuum. The crude product obtained was purified on silica gel column chromatography (solvents, ratio?), to obtain white crystalline product diphenylamine 3a (1.60 g) with 95percent yield. All reactions were similarly carried out.
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