Synthetic Route of 14618-78-1, These common heterocyclic compound, 14618-78-1, name is 4,4-Dimethoxybutanenitrile, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
SYNTHESIS EXAMPLE 4 Production of methyl 4,5,7-trichloroindole-3-acetate: 10.0 Grams (0.047 mole) of 2,4,5-trichlorophenylhydrazine, 9.2 g (0.07 mole) of beta-cyanopropionaldehyde dimethylacetal and 7.1 g (0.052 mole) of zinc chloride were mixed and then heated in a nitrogen stream at 140 C. for 2 hours. The reaction mixture was cooled to room temperature and dissolved in an acetic acid-water (2:1) solution, and the resulting solution was extracted with ethyl acetate. The ethyl acetate phase was washed with a saturated aqueous sodium bicarbonate solution, water and then a saturated aqueous sodium chloride solution, and then dried over anhydrous sodium sulfate. The ethyl acetate was removed by distillation under reduced pressure to obtain a black oily substance, which was then purified by a silica gel column chromatography to obtained 0.86 g of the desired compound represented by the formula: STR15 The analysis result of NMR of this compound is shown below. 1 H NMR (200 MHz) (CD3)2 CO, TMS) ppm: 7.48 (1H, s).. C2 –H 7.34 (1H, s).. C6 –H 3.99 (2H, s).. CH2 — 3.66 (3H, s).. OCH3 MS (75 ev) (relative intensity, %) m/z 295 (M+ +4, 10), 293 (M+ +2, 23), 291 (M+, 24), 260 (6), 259 (5), 258 (7), 236 (30), 234 (91), 232 (100), 199 (7), 198 (9), 197 (11), 162 (12), 161 (13), 118 (7), 116 (8), 97 (9), 98 (9).
The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Nippon Kayaku Kabushiki Kaisha; US4806143; (1989); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts