Method for synthesis of N-alkyl carbazole and derivatives thereof
一种烷基咔唑、四氢咔唑的技术，应用在合成N-烷基咔唑及其衍生物领域，能够解决烷基咔唑收率和纯度低等问题
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Embodiment 1
[0058] Preparation of 2-chlorocyclohexanone
[0059] 490 g of cyclohexanone was added to water (1250 ml) to obtain a mixed solution. Mixed solution in a 4 liter capacity integrated reactor and in 20 0 Under strong stirring at C, the reactor includes a mechanical stirrer, the inlet of the sealing liquid pipe for adding chlorine, a thermocouple and a fractional distillation condenser. Then, while vigorously stirring, chlorine gas was passed in at a rate of 71 g / h for 4 hours to precipitate the reaction mixture. The bottom organic layer was separated from the upper aqueous layer and washed with Na 2 CO 3 The solution neutralized the precipitate to give an oily layer. The mixed oily layer contained 436 g of 2-chlorocyclohexanone, 102 g of cyclohexanone and 54 g of dichloride.
[0060] Yield of 2-chlorocyclohexanone: 82%, purity > 98% by gas chromatography (GC).
Embodiment 2
[0062] Preparation of 9-ethyl-1,2,3,4-tetrahydrocarbazole
[0063] 266.2 g of N-ethylaniline were charged to a reactor equipped with a mechanical stirrer, thermocouples and a double coil condenser with chilled water circulating over the Dean-Stark apparatus. After 1 hour, 132.5 g of 2-chlorocyclohexanone was added to the reactor to obtain a reaction product, which was heated to 100 0 C and stirred for 2 hours. Continue to heat the reaction product to 150-160° C., and stir for another 2 hours when exotherm is seen. Water produced in the reaction was removed by vacuum from the top of the condenser (equipped with chilled water circulation), ideally until water collected on the side of the Dean-Stark unit. Wash with funnel, hydrochloric acid and water to remove excess N-ethylaniline. The resulting organic layer was washed to remove the acid, and concentrated under reduced pressure to obtain 178.2 g of mucus with a GC purity of 98.4% (yield 89%). The mass spectrum matched the...
Embodiment 3
[0068] 266.2 g of N-ethylaniline and 200 ml of o-xylene were simultaneously added to the reactor. After 2 hours, 132.5 g of 2-chlorocyclohexanone was added to obtain a clear solution, which was then heated to 100 0 C and stirred for 2 hours to remove water. Heat the mixture further to 150 - 160 0 C, while applying a little vacuum to remove moisture. The reaction product was subjected to the above process to obtain 136 g of crude 9-ethyltetrahydrocarbazole with a GC purity of 96.8%.
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