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ChemicalBook CAS DataBase List 6-METHYLTETRALINE
1680-51-9

6-METHYLTETRALINE synthesis

13synthesis methods
2-Methylnaphthalene

91-57-6

2-methyltetralin

3877-19-8

6-METHYLTETRALINE

1680-51-9

The general procedure for the synthesis of the target compounds (CAS: 3877-19-8) and 6-methyl-1,2,3,4-tetrahydronaphthalene from 2-methylnaphthalene is as follows: first, n-hexadecane solution of the model feedstock is prepared, where the substrate concentration is 10% (the substrate consists of unsubstituted bicyclic aromatic naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, 1,5-dimethylnaphthalene and 2,3-dimethylnaphthalene). The substrate and a calculated amount of precursor compound were accurately weighed and added to the insert tube, adding the oxide or its precursor (e.g., zirconium oxide) if necessary. Subsequently, the insert tube was placed in a 20 mL steel autoclave. The reaction conditions were set at temperatures ranging from 380°C to 400°C, hydrogen pressures ranging from 2 MPa to 5 MPa, and strong stirring was maintained. The molar ratios were set as follows: substrate/Mo 18.4:1 and 36.8:1, substrate/W 18.4:1, substrate/Ti 2.4:1, 4.9:1, 7.3:1, 9.7:1, and 12.5:1, substrate/Al 4.9:1 and 9.7:1, substrate/Zr 70.2:1, and substrate/Co 37.2:1. Catalysts were prepared by in-situ sulfidation in hydrocarbon feedstock prepared by in situ sulfurization in hydrocarbon feedstock with the addition of elemental sulfur (dissolved in n-hexadecane) in an amount of 2.5 wt% by weight of the feedstock. The autoclave was heated to the experimental temperature at a rate of 10°C/min. Upon completion of the reaction, the autoclave was cooled to room temperature and the catalyst was separated from the conversion product by centrifugation. Non-uniformity of the gaseous products of feedstock conversion was observed during the experiment.

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Yield: 64.8% , 27.8%

Reaction Conditions:

with aluminum oxide;hydrogen;molybdenum hexacarbonyl in Hexadecane at 400; under 15001.5 Torr; for 2 h;Autoclave;Reagent/catalyst;

Steps:

Catalyst Testing and Product Analysis Procedures
General procedure: Model feedstocks were 10% solutions of substrates(the bicyclic aromatic HCs unsubstituted naphthalene,1- and 2-methylnaphthalenes, and 1,5- and 2,3-dimethylnaphthalenes) in n-hexadecane. A weighedamount of a substrate, as well as a calculated amountof the precursor compounds, was introduced into aninsert tube, while adding oxides or their precursors (inthe case of zirconium oxide) where necessary. Then the insert was placed into a 20-mL steel autoclave. Theexperiments were conducted at 380 and 400° and ahydrogen pressure of 2 and 5 MPa under intense stirring.The molar ratios were as follows: substrate/Mo of18.4 : 1 and 36.8 : 1, substrate/W of 18.4 : 1, substrate/Ti of 2.4 : 1, 4.9 : 1, 7.3 : 1, 9.7 : 1, and 12.5 : 1,substrate/Al of 4.9 : 1 and 9.7 : 1, substrate/Zr of70.2 : 1, substrate/Co of 37.2 : 1, and substrate/Ni of37.2 : 1. The catalysts were sulfided in situ in thehydrocarbon raw materials by adding elemental sulfurin the amount of 2.5 wt % relative to the weight of theraw materials (a solution of a substrate in n-hexadecane).The autoclave was heated to the temperature ofthe experiment at a rate of 10 deg/min. Upon the completionof the experiment, the autoclave was broughtup to room temperature and the catalyst was separatedfrom the conversion products via centrifugation. Noformation of the gaseous products of the conversion ofthe raw materials was observed.

References:

Zakharyan;Onishchenko;Maksimov [Petroleum Chemistry,2018,vol. 58,# 1,p. 22 - 31][Neftekhimiya,2018,vol. 58,# 1,p. 26 - 35,10]

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