25127-31-5Relevant articles and documents
Synthesis of dibenzocycloketones by acyl radical cyclization from aromatic carboxylic acids using methylene blue as a photocatalyst
Jiang, Hongshuo,Mao, Guijie,Wu, Hongfeng,An, Qi,Zuo, Minghui,Guo, Weihao,Xu, Chunzhao,Sun, Zhizhong,Chu, Wenyi
, p. 5368 - 5373 (2019)
An efficient intramolecular radical cyclization reaction via photoredox catalysis was developed for the synthesis of dibenzocycloketone derivatives using methylene blue as a photosensitizer. This strategy could be widely used to synthesize large heterocycles due to the unique reactivity of phosphoranyl radicals formed by a polar/SET crossover between an aromatic carboxylic acid and a phosphine radical cation. Attractive features of this process include generation of an acyl radical by an inexpensive and metal-free photocatalyst, which effectively undergoes a cyclization process.
Improved synthesis method of doxepin hydrochloride
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, (2021/11/19)
The invention relates to an improved synthesis method of doxepin hydrochloride. The method comprises the following steps: (1) reacting triphenylphosphine with 3 - chlorine -1 - (N, N - dimethyl) propylamine to prepare (3 - (dimethylamino) propyl) triphenyl phosphine chloride. (2) Reaction of (3 - (dimethylamino) propyl) triphenyl phosphine chloride and 6, 11 -dihydrodibenzo [b, e] oxepin -11 - ketone under a strong base condition to Wittig prepare a doxorubicin. (3) The multi-plug is subjected to salt formation reaction with hydrochloric acid to prepare the doxorubicin hydrochloride. The second Reaction is adopted in Wittig-step reaction, so that the reaction is simpler, the requirements for water and reaction equipment of the solvent and the raw materials are lower, and the repetition rate is higher. Compared with the prior art, the method has the advantages of simple process, low production cost, less process steps and the like.
Synthetic method of doxepin hydrochloride
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Paragraph 0036; 0047-0049; 0054-0055; 0060-0061; 0066-0067, (2020/12/30)
The invention discloses a synthetic method of doxepin hydrochloride. The synthetic method comprises the following steps: using N, N-dimethyl-3-chloropropylamine as an initial raw material, carrying out Grignard reaction, carrying out addition reaction on the reaction product and 6, 11-dihydrodibenzo [b, e] oxepine-11-ketone, and sequentially carrying out elimination reaction and salifying reactionto synthesize the final product. According to the method, high-purity doxepin hydrochloride can be obtained through four-step synthesis, a substitution reaction is not needed, and the yield of the prepared product is high. Compared with the existing synthesis process, the method has the advantages of few synthesis steps, simple process, short production period, low cost and the like.