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.597-31-9, name is 3-Hydroxy-2,2-dimethylpropanal, molecular formula is C5H10O2, molecular weight is 102.1317, as common compound, the synthetic route is as follows.Computed Properties of C5H10O2
EXAMPLE 2 (COMPARATIVE EXPERIMENT)Hydrogenation of the HPA-Comprising Stream from Example 1The HPA-comprising stream used was the mixture prepared according to example 1.This HPA-comprising stream was first passed into a hydrogenation reactor which was operated in trickle mode at H2 pressure 37-40 bar and at 100-120 C. The hourly space velocity was 0.28 kg of solution/(1 cat.*h). The catalyst used was a Cu/Al2O3 catalyst as described in EP-A-44444 or WO-A-2007/042456, which was activated according to the disclosure of EP-A-44444 or WO-A-2007/042456 in a tubular reactor at 190 C. at ambient pressure by passing a mixture of 5% by volume of hydrogen and 95% by volume of nitrogen (total volume 50 1 (STP)/h) over it for 24 h.The hydrogenation discharge was split into two substreams.In steady-state operation, one substream as the NPG-comprising circulation stream was combined with the HPA-comprising stream.The ratio of NPG-comprising circulation stream to the HPA-comprising stream from example 1 was approx. 10:1.The composition of the circulation stream was 25% by weight of water, 68% by weight of NPG, 1.6% by weight of HPA, remainder (approx. 6% by weight) other organic compounds.The hydrogenation feed thus obtained was subsequently introduced into the hydrogenation reactor.The composition of the hydrogenation feed was 25% by weight of water, 64% by weight of NPG, 7% by weight of HPA and 4% by weight of other organic compounds.The weight ratio of HPA to NPG in the hydrogenation feed was approx. 1:9.The portion of the hydrogenation discharge which was not recycled as the NPG-comprising circulation stream was conducted through a second hydrogenation reactor.The second hydrogenation reactor was operated at 37-40 bar and a temperature of 110-130 C. The catalyst used was the same catalyst as in the first hydrogenation reactor.A pH of approx. 8 was established in the discharge of the second reactor, by adding trimethylamine (TMA) (pH regulator) to the HPA-comprising stream from example 1.The pH regulator was supplied before the combination of the HPA-comprising stream with the NPG-comprising circulation stream.The temperature of the HPA-comprising stream from example 1 on supply of the pH regulator (TMA) was 80 C. The residence time between the addition of the pH regulator and the supply of the circulation stream was 10 minutes (>5 minutes).EXAMPLE 3 (INVENTIVE EXAMPLE)Hydrogenation of the HPA-Comprising Stream from Example 1The hydrogenation was effected under the same conditions as in example 2. To establish a pH of 8 at the outlet of the second reactor, the pH regulator (TMA) was, however, supplied directly to the NPG-comprising circulation stream before the NPG-comprising stream was combined with the HPA-comprising stream from example 1. The weight ratio of HPA to NPG in the hydrogenation feed obtained by combining these streams was approx. 1:9.The composition of the hydrogenation feed was 25% by weight of water, 64% by weight of NPG, 7% by weight of HPA and 4% by weight of other organic compounds.
At the same time, in my other blogs, there are other synthetic methods of this type of compound,597-31-9, 3-Hydroxy-2,2-dimethylpropanal, and friends who are interested can also refer to it.
Reference:
Patent; BASF SE; US2011/282106; (2011); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts