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3074-77-9

3-Ethyl-4-methylhexane synthesis

4synthesis methods
-

Yield:589-53-7 11% ,52896-91-0 70%

Reaction Conditions:

with hydrogen at 220; for 7 h;

Steps:

3

The Ir-ReOx/Si02 catalyst was prepared using the published method [Chen et a., ChemSiisChem 2013, 6, 613] and reactions were carried out in batch mode as described above for the Cu-ZnO/AJ2( system, except that a range of temperatures between 200 and 300 °C were studied. The results for the deoxygenation of ALD 3 are shown in Table 1. Starting at the same temperature as used for Cu-ZnO/AbO:?, an improved yield of 72% hydrocarbons was observed using the Ir-ReOx/SiCh catalyst. A considerable degree of C-C bond cleavage was seen, as was the case with the copper-zinc catalyst, which prompted attempts to perform the hydrogenation at lower temperatures. As shown in Table I, reduction of the reaction temperature first to 2.40 and then 2.20 °C increased selectivity for the Cio product, i.e. the product which would result if no C-C bond cleavage occurred, while increasing the overall hydrocarbon yield up to 88%. Decreasing the reaction time (not shown) or the reaction temperature (200 °C) was found to substantially lower the yield of hydrocarbons. Table 1. Angelica lactone dimer 3 conversion and hydrocarbon yield with different catalytic systems. Temp. Time Conv. Hydroc Yield (%)a Catalyst (CC) (h) (%) c7 c8 c. fetal Cu-ZnO/Al2( + γ- 300 100 3 12 5 21 41 A1203 Cu-ZnO/Al20, + 300 3 100 15 35 14 68 HPW/MCM-41" Ir-ReCVSiOz 300 3 100 16 19 33 72 fr-ReOx/Si02 240 6 100 13 10 60 84 Tx-ReOx/SiG2 220 1 100 1 1 1 6 70 88 Tx-ReOx/Si02 200 100 0 6 1 10 Pt-ReOx/C 240 6 100 2 8 18 60 88 Pt-ReOx/C 220 100 z 4 7 13 26 Pt-WOx/A]203 240 6 100 1 10 19 aMolar %C yields as determined by GC-MS integration against -alkane standards. '2Gt% 12-phosphotungstic acid (HPW) loaded on mesoporous silica (MCM-41).

References:

WO2015/73889,2015,A1 Location in patent:Paragraph 0097

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