Synthetic Route of 72291-30-6, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, This compound has unique chemical properties. The synthetic route is as follows.
The reactant and the catalyst are initially charged in the autoclave and the contents are inertized by purging with nitrogen. Subsequently, 5 bar of hydrogen are injected. The desired amount of ammonia is metered in and then the autoclave is heated slowly with stirring to the reaction temperature (80 C.). This step takes an average of 90 min, i.e. the delay time of the reactant solution in contact with ammonia is approx. 90 min. On attainment of the reaction temperature, hydrogen is injected rapidly to the pressure specified in Table 1 below and consumed hydrogen is replaced by metering under pressure control over the experiment time until no further hydrogen absorption is recorded.The autoclave experiments are carried out in a 2.5 l autoclave with hollow-shaft disk stirrer (stirrer speed approx. 600 rpm), electrical heating and jacket air cooling, 2 baffles, sparging through the autoclave lid and introduction of the hydrogen via the hollow-shaft stirrer. The weights for Raney catalysts are corrected for 10% water moisture, i.e., in real terms, 10% more water-moist catalyst is weighed out than specified. Reaction effluents are analyzed via gas chromatography (GC) (conditions: 60 m DB1701; internal diameter 0.32 mm; film thickness 0.25 mum; detector: FID; temperature program: 80 C.?10 K/min?280 C., 40 min, split ratio 100:1, carrier gas helium) and the compositions are reported in % by weight.The reactor yield is determined by means of gas chromatography with internal standard (I.S.) (I.S. piperidine; the concentration thus obtained in the crude effluent is multiplied by the total mass of the crude effluent and the yield thus calculated is compared to the theoretical yield). The reactions are all carried out with methyl 2-cyano-2,2-dimethylacetate with a purity of >99.8%. The main product obtained is aminopivalinamide (3-amino-2,2-dimethylpropionamide). TABLE 1 Pressure/ % by weight ConcentrationNH3/ Purity Conversion Reactor Example bar Catalyst of catalyst Solvent % nitrile (crude, GC) % % yield % 1 200 Ra-Ni 10 NMP 30 20:1 98.7 100 not determined 2 65 Ra-Co 10 BuOH 40 7.7:1 98.8 100 94.0% 3 65 Ra-Ni 10 BuOH 40 7.7:1 98.2 99.7 90.6% 4 65 Ra-Ni 2.5 BuOH 40 3:1 93.7 99.7 84.9% 5 65 Ra0Co 2.5 BuOH 40 3:1 94.9 99.9 86.7 6 65 Ra-Co 5 MeOH 40 3:1 96.5 99.1 90.4 7 65 Ra-Co 5 MeOH 40 3:1 96.6 99.1 91.1 8 65 Ra-Co 5 BuOH 40 3:1 90.0 99.4 88.2 The examples show that very good selectivities of at least 90% are achievable with Raney nickel and Raney cobalt. The higher the amount of ammonia, the higher the catalyst concentration and the higher the hydrogen pressure, the better is the selectivity. In example 8, a metal determination is carried out, 430 ppm of Co are found in the reaction effluent.
The chemical industry reduces the impact on the environment during synthesis Methyl 2-cyano-2-methylpropanoate. I believe this compound will play a more active role in future production and life.
Reference:
Patent; BASF SE; US2008/306299; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts