Method for subjecting acetylene and ketone compound to addition reaction

Abstract

The invention discloses a method for subjecting acetylene and a ketone compound to an addition reaction. The method comprises the following steps: (1) providing a continuous reaction device, wherein the continuous reaction device comprises multiple bubbling tubular reactors which are arranged in series, and the multiple bubbling tubular reactors are connected through connection pipes; (2) sendinga raw material solution containing the ketone compound and an alkali into the multiple bubbling tubular reactors; and (3) at normal pressure, bubbling the acetylene from the bottom of the first bubbling tubular reactor to carry out the addition reaction. According to the technical scheme, by adopting the method for subjecting the acetylene and the ketone compound to the addition reaction, the acetylene and the ketone compound are reacted in the multiple bubbling tubular reactors which are arranged in series, enough gas-liquid contact time can be guaranteed, thus acetylene gas can be fully used, the utilization rate of the acetylene gas is improved, the usage amount of the acetylene is effectively reduced, and not only is the cost reduced, but also the safety is further improved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for addition reaction of acetylene and ketone compounds. Background technique [0002] Acetylene is a colorless, flammable gas with an aromatic odor. The flash point is -17.78°C, and the spontaneous ignition point is 305°C. The explosion limit in air is 2.3% to 72.3%. In liquid and solid state, or in gaseous state and under a certain pressure, there is a danger of violent explosion. Factors such as heat, vibration, and electric sparks can cause an explosion. [0003] The addition reaction between acetylene and ketones is a very important reaction in the field of organic synthesis. For example, a key step in the synthesis of a potential anti-HIV agent, 3',4'-Di-O-(-)-camphanoyl-(+)-cis-khellacton (DCK, deoxycytidine kinase), is Addition reaction of acetylene gas with ketone under the action of strong base. Acetylene is an extremely flammable gas, and there ...

AI Technical Summary

Problems solved by technology

However, this process method still requires the use of acetylene gas, so there is also a great potential safety hazard in the scale-up production process

However, if the ethynyl format reagent is directly purchased, the process cost will inevitably increase exponentially due to the high cost of the ethynyl format reagent.

[0005] In addition, in the traditional batch reaction process, when carrying out industrial production, the reaction tank is usually more than several thousand liters, and the reaction volume is huge

Moreover, the structural design of the traditional batch reactor is not suitable for the gas-liquid two-phase reaction under normal pressure. During the reaction process, it is necessary to pass acetylene gas into the reaction system all the time.

There is a large excess of acetylene gas, the utilization rate is low, and it is easy to make acetylene accumulate in the reaction kettle and the reaction pipeline, which poses a great safety hazard

Images