Benzo cyclohepten derivate, and preparation and medical use thereof
A technology for benzocycloheptene and medicinal salts, applied in the fields of benzocycloheptene derivatives, their preparation and medical use, can solve problems such as high toxicity and many complications
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Embodiment 1
[0190] Example 1: N-[3-(2-diethylaminoethoxy)-4-methylphenyl]-3-(4-methylphenyl)-8,9-dihydro-7H-benzene Preparation of cycloheptene-6-carboxamide
[0191]
[0192] a. Methyl 4-(4-bromobenzoyl)butyrate
[0193] Bromobenzene (150ml) and aluminum chloride (0.3mol) were placed in a 250ml three-necked flask, and glutaric acid monomethyl chloride (0.14mol) was slowly added dropwise under ice-cooling, and reacted at room temperature for 3.5 hours, and the reaction mixture was poured into a mixture of hydrochloric acid and ice, and the organic phase was separated. The aqueous phase was extracted with ethyl acetate, and the combined organic phases were washed with water and saturated brine. Dry over anhydrous magnesium sulfate, filter, and evaporate most of the bromobenzene under reduced pressure to obtain 39.1 g of a yellow oil with a yield of 98%. It was directly used in the next reaction without purification.
[0194] b. 4-(4-Bromobenzoyl)butanoic acid
[0195] The yellow...
Embodiment 2
[0216] Example 2: N-[3-(2-diisopropylaminoethoxy)-4-methylphenyl]-3-(4-methylphenyl)-8,9-dihydro-7H- Preparation of Benzocycloheptene-6-Carboxamide
[0217]
[0218] a. Diisopropyl-[2-(2-methyl-5-nitrophenoxy)ethyl]amine
[0219] Using the method for preparing diethyl-[2-(2-methyl-5-nitrophenoxy)ethyl]amine in Example 1, the N,N-diethylethylamine in Step j of Example 1 The amine hydrochloride was replaced with N,N-diisopropylethylamine hydrochloride to give a yellow oil. MS [M] + = 280.4 m / e.
[0220] b. 3-(2-Diisopropylaminoethoxy)-4-methylamine
[0221] Using the method for preparing 3-(2-diethylaminoethoxy)-4-methylaniline in Example 1, diethyl-[2-(2-methyl-5 -Nitrophenoxy)ethyl]amine was replaced by diisopropyl-[2-(2-methyl-5-nitrophenoxy)ethyl]amine from step a above to give a colorless oil . MS [M] + = 250.4 m / e.
[0222] c. N-[3-(2-Diisopropylaminoethoxy)-4-methylphenyl]-3-(4-methylbenzene base)-8,9-dihydro-7H-benzocycloheptene-6-carboxamide
[0223] ...
Embodiment 3
[0224] Example 3: N-[3-(2-dimethylaminoethoxy)-4-methylphenyl]-3-(4-methylphenyl)-8,9-dihydro-7H-benzene Preparation of cycloheptene-6-carboxamide
[0225]
[0226] a. Dimethyl-[2-(2-methyl-5-nitrophenoxy)ethyl]amine
[0227] Using the method for preparing diethyl-[2-(2-methyl-5-nitrophenoxy)ethyl]amine in Example 1, the N,N-diethylethylamine in Step j of Example 1 The amine hydrochloride was replaced with N,N-dimethylethylamine hydrochloride to give a yellow oil. MS[M]+=224.3m / e
[0228] b. 3-(2-Dimethylaminoethoxy)-4-methylaniline
[0229] Using the method for preparing 3-(2-diethylaminoethoxy)-4-methylaniline in Example 1, diethyl-[2-(2-methyl-5 -Nitrophenoxy)ethyl]amine was replaced with dimethyl-[2-(2-methyl-5-nitrophenoxy)ethyl]amine from step a above to give a colorless oil. MS[M]+=194.3m / e
[0230] c. N-[3-(2-Dimethylethoxy)-4-methylphenyl]-3-(4-methylphenyl)-8,9- Dihydro-7H-benzocycloheptene-6-carboxamide
[0231] Using the preparation method of step...
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