Reference of 72291-30-6, A common heterocyclic compound, 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, molecular formula is C6H9NO2, 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.
The experiment examples are carried out in a 1 l reactor (10×2000 mm), equipped with feed pumps for solvent, ammonia and nitrile ester, charged with 250 ml of steel rings in the lower and upper reactor section, and centrally with 500 ml of tablets (5×3 mm) of a hydrogenation catalyst of the following composition: 28% NiO, 28% CoO, 13% CuO and 31% ZrO2, in liquid phase mode. The reduction procedure of the catalyst is as follows: the reactor is heated to 180 C. at a hydrogen feed of 50 l/h within 5 hours, then kept at 180 C. with 50 l/h of hydrogen for 20 hours, cooled under hydrogen and purged with MeOH, before ammonia and reactant and also solvent are fed in. The steel rings in the lower part of the reactor serve as the delay time zone for the amidation. 11 equivalents of hydrogen are fed in per nitrile used. The delay time is thus approx. 10 minutes. Example 10250 g/h of tetrahydrofuran (THF) and methyl 2-cyano-2,2-dimethylacetate as the nitrile ester (in a weight ratio of 70:30) and 205 g of ammonia (20 equivalents of ammonia based on nitrite ester) are conducted through the reactor at 200 bar and 100 C. The volume space velocity is 0.15 kg/l*h. The effluent analysis shows (calculated without solvent) 33.083% aminopivalinamide, 65.68% methyl aminopivalate and 0.49% others. The delay time is approx. 27 minutes.
The synthetic route of 72291-30-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BASF SE; US2008/306299; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts