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[urri]

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Посмотрите,пожалуйста,получение

Nc1cccc2ncncc12

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[mishka]

из хлорзамещенного


With 4,4'-dimethyl-2,2'-bipyridine; nickel diacetate; ammonium bromide; 1,8-diazabicyclo[5.4.0]undec-7-ene In tetrahydrofuran; dimethyl sulfoxide at 85℃; Irradiation; Inert atmosphere;
73 %
Song, Geyang; Nong, Ding-Zhan; Li, Qi; Yan, Yonggang; Li, Gang; Fan, Juan; Zhang, Wei; (…) Xiao, Jianliang; Xue, Dong
[ACS Catalysis, 2022, vol. 12, # 24, p. 15590 - 15599]



With hexaamminenickel (II) chloride; 4,4'-dimethyl-2,2'-bipyridine; 1,8-diazabicyclo[5.4.0]undec-7-ene In tetrahydrofuran; dimethyl sulfoxide at 85℃; Irradiation; Inert atmosphere; Sealed tube;
73 %
Song, Geyang; Song, Jiameng; Li, Qi; Nong, Ding-Zhan; Dong, Jianyang; Li, Gang; Fan, Juan; Wang, Chao; Xiao, Jianliang; Xue, Dong
[Angewandte Chemie - International Edition, 2024, vol. 63, # 6, art. no. e202314355][Angew. Chem., 2024, vol. 136, # 6]

из 4-Chlor-5-nitro-chinazolin

With Lindlar's catalyst; 2-methoxy-ethanol Hydrogenation.und anschliessenden Dehydrierung mit wss.K3;
Osborn et al.
[Journal of the Chemical Society, 1956, p. 4191,4205]

With Lindlar's catalyst; 2-methoxy-ethanol Hydrogenation.und anschliessend Dehydrierung mit Palladium/Kohle;
Naff; Christensen
[Journal of the American Chemical Society, 1951, vol. 73, p. 1372]

тамже стадия из 5-Nitro-4-oxo-3,4-dihydro-chinazolin описана


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With [2,2]bipyridinyl; hexaamminenickel (II) chloride; 1,8-diazabicyclo[5.4.0]undec-7-ene In dimethyl sulfoxide at 85℃; Inert atmosphere; Irradiation;

Experimental Procedure
73 %
Current Patent Assignee: SHAANXI NORMAL UNIVERSITY - CN115650883, 2023, A
Location in patent: Paragraph 0016-0019; 0072-0075


Abstract
15 Example 1
General procedure: In an argon atmosphere, add 38.1 mg (0.2 mmol) 4-chlorophenyl methylsulfone, 16.2 mg (0.07 mmol) nickel-amine complex [(NH3)6Ni]Cl2 , 1.9mg (0.01mmol) bipyridine, 45.6mg (0.3mmol) DBU, 2mL dimethyl sulfoxide and magneton were added to the reaction tube, and the reaction was carried out at 85 °C for 24 hours under 390~395nm purple light. After the reaction, it was cooled to room temperature, saturated sodium chloride aqueous solution and ethyl acetate were added to dilute and extract to obtain organic phase, vacuum distillation was obtained crude product, a mixture of petroleum ether and ethyl acetate volume ratio of 3:1 to 1:2 was used as an eluent, and the column chromatography separation product was obtained to obtain white solid p-aminobenzyl sulfone with the following structural formula, and its yield was 90%

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