2,6-Lutidine synthesis

9synthesis methods

Product Name:2,6-Lutidine
CAS Number:108-48-5
Molecular formula:C7H9N
Molecular Weight:107.15

Synthesis from ethyl acetoacetate, formaldehyde and ammonia; isolated from basic fraction of coal tar

504-03-0 Synthesis

504-03-0
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108-48-5
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$9.90/190μL

Yield:108-48-5 >99 %Chromat.

Reaction Conditions:

in octane at 120; under 760.051 Torr; for 18 h;Inert atmosphere;Schlenk technique;

Steps:

Typical procedure for the acceptorless dehydrogenation of cyclic amines:

General procedure: Into a Schlenk tube (volume: ca. 20 mL) connected to a balloon partially filled with Ar gas, Pd/LDH (75 mg, Pd: 3 mol %), 4-isopropylpiperidine (0.5 mmol), decane (internal standard, 0.1 mmol), octane (2.0 mL), and a Teflon-coated magnetic stir bar were successively placed, and the reaction mixture was vigorously stirred at 120 °C, in 1 atm of Ar. After the reaction was completed, the conversion of 4-isopropylpiperidine and the yield of 4-isopropylpyridine were determined by GC analysis. The reactions of piperidine and 4-methylpiperidine were conducted in a test tube with an Ar balloon. During these reactions, the upper side of the test tube was cooled by refrigerant (-5 °C).

References:

Oyama, Takashi;Yatabe, Takafumi;Jin, Xiongjie;Mizuno, Noritaka;Yamaguchi, Kazuya [Chemistry Letters,2019,vol. 48,# 6,p. 517 - 520] Location in patent:supporting information