Octanoic acid, 3,7-dimethyl-6-octenyl ester synthesis

Yield:72934-05-5 90%

Reaction Conditions:

in tetrahydrofuran; for 3 h;

Steps:

5 Embodiment 5

Takes bitterly 28.8 g (0.2 μM), adding thionyl chloride 17.85 g (0.15 μM), mixing after the 60 °C reaction 3 hours, adding containing 15.6 g (0.1 μM) Citronellol tetrahydrofuran solution 20 ml, continue to reaction 3 hours, the reaction solution NaOH solution is adjusted to pH 6 - 7, separating the organic layer, the aqueous layer extracted with ethyl acetate, the combined organic layer, saturated salt water for, water-free Na₂ SO₄ Drying overnight, the solvent, column chromatography (silica gel 200 - 300 mesh), b petroleum ether and ethyl acetate (15:1) as eluent, steam in addition to the eluant, to obtain colourless liquid 259.4 g, yield: 90%. The product of the 1 HNMR and MS data as follows: ESI - MS m/z: 281.4 [M + 1] +; 1 H NMR (500 MHz, CDCl₃ ): Δ 5.10 (t, J=7. 5 Hz, 1 H), 3.68 (m, 2 H), 2.3 - 1.8 (m, 16 H), 1.68 (s, 3 H), 1.60 (s, 3 H), 1.7 - 1.52 (m, 3 H), 1.4 - 1.1 (m, 3 H), 0.91 (d, J=6. 5 Hz, 3 H).

References:

CN107353203,2017,A Location in patent:Paragraph 0049; 0050