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[ CAS No. 5346-21-4 ] {[proInfo.proName]}

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Chemical Structure| 5346-21-4
Chemical Structure| 5346-21-4
Structure of 5346-21-4 * Storage: {[proInfo.prStorage]}
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Product Details of [ 5346-21-4 ]

CAS No. :5346-21-4 MDL No. :
Formula : C13H11NO Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 197.23 Pubchem ID :-
Synonyms :

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Application In Synthesis of [ 5346-21-4 ]

* 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.

  • Upstream synthesis route of [ 5346-21-4 ]
  • Downstream synthetic route of [ 5346-21-4 ]

[ 5346-21-4 ] Synthesis Path-Upstream   1~1

  • 1
  • [ 5346-21-4 ]
  • [ 15679-03-5 ]
YieldReaction ConditionsOperation in experiment
91% With thionyl chloride; sulfuryl dichloride; titanium tetrachloride In toluene at -10 - 0℃; Reflux Reaction flask was added Intermediate I (41.6g, 0.21mol) and 100mL of toluene, and stirred and dissolved; In another reaction flask, the sulfonyl chloride (43g, 0.32mol), thionyl chloride (74g, 0.63mol )And titanium tetrachloride (80g, 0.42mol) were mixed and cooled to -10 ~ 0 , and then a toluene solution of Intermediate I was slowly added to the system, the system was maintained during the addition at -10 ~ 0 ;After joining,The system is heated to reflux and the reaction 18-24h, sulfur dioxide and hydrogen chloride escapes, the reaction was monitored by HPLC process; when HPLC showed that the system of Intermediate I content of less than 1percent, heating was stopped,The reaction mixture was added dropwise to a mixture of aqueous ammonia and water at -10 to 0 ° C, and the mixture was stirred at room temperature for 2 hours. Control the rate of drop to ensure that the system termination temperature of -10 ~ 0 . The organic phase was concentrated and recrystallized from n-heptane to give 40.7 g of 6-chlorophenanthrene in a yield of 91percent and a purity of 99.5percent. The filtrate was concentrated under reduced pressure, and the filtrate was concentrated to dryness.
Reference: [1] Patent: CN105906565, 2016, A, . Location in patent: Paragraph 0051; 0052; 0053
[2] Journal of the Chemical Society, Chemical Communications, 1995, # 22, p. 2295 - 2296
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