Electric Literature of 144-19-4, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.144-19-4, name is 2,2,4-Trimethyl-1,3-pentanediol, molecular formula is C8H18O2, molecular weight is 146.2273, as common compound, the synthetic route is as follows.
EXAMPLE 1 Preparation of 1-(2-methyl-2-propenyloxy)-2,2,4-trimethylpentan-3-ol: To a 1L flask equipped with a reflux condenser and a thermometer, was added 292.5 g (2.0 mol) of 2,2,4-trimethylpentan-1,3-diol, 352.0 g (4.4 mol) of 50% aqueous NaOH, and 6.45 g (20 mmol) of tetrabutyl ammonium bromide.This mixture was heated in an oil bath and when the reaction mixture reached 50 C., 199.2 g (2.2 mol) of methallyl chloride was added drop-wise over 50 minutes.During the addition, the oil bath temperature was gradually raised to 100 C. and the reaction was continued for an additional 3 hours at 100 C. The reaction mixture was cooled, quenched with 400 ml of water, and extracted twice with 100 ml of toluene.The combined organic layers were washed with 50 ml of saturated ammonium chloride and 50 ml of saturated sodium chloride and evaporated to give 408 g of crude 1-(2-methyl-2-propenyloxy)-2,2,4-trimethylpentan-3-ol.After reduced pressure distillation (71-80 C., 3 MmHg), 377.1 g (yield 94.1%) of 1-(2-methyl-2-propenyloxy)-2,2,4-trimethylpentan-3-ol was obtained. 1H-NMR (500 MHz, CDCl3, delta) ppm: 0.93 (d, J=6.8 Hz, 3H), 0.95 (s, 3H), 0.96 (s, 3H), 1.02 (d, J=6.9 Hz, 3H), 1.74 (s, 3H), 1.85-1.94 (m, 1H), 3.13 (d, J=3.8 Hz, 1H), 3.19 (d, J=8.7 Hz, 1H), 3.38-3.43 (m, 2H), 3.85 (s, 2H), 4.88 (s, 1H), 4.91 (s, 1H). IR (film) cm-1: 3501, 3077, 2961, 2873, 1657, 1472, 1455, 1414, 1369, 1259, 1171, 1093, 1032, 992, 899. [0042] MS (m/e): 200 (M+), 183, 167, 157, 145, 128, 110, 95, 85, 83, 73, 55, 43, 29.
Statistics shows that 144-19-4 is playing an increasingly important role. we look forward to future research findings about 2,2,4-Trimethyl-1,3-pentanediol.
Reference:
Patent; Takasago International Corporation; US2004/14633; (2004); A1;,
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