58566-44-2Relevant articles and documents
Preparation method of organic intermediate N, N-bis (beta-ethoxyl) benzamide
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Paragraph 0011-0015, (2020/04/02)
The invention discloses a preparation method of N, N-bis (beta-ethoxyl) benzamide. The preparation method comprises the following steps: step 1, preparing materials: preparing methyl benzoate, N, N-diethanol amine, a catalyst and a mixed solvent according to a mass ratio of 1: (0.77-1.16): (0.011-0.055): (1.10-2.57), taking the methyl benzoate and the N, N-diethanol amine as raw materials, and stirring to obtain a mixed solution; and performing a condensation reaction in the presence of the catalyst, wherein the condensation reaction temperature is 80-95 DEG C, and the condensation reaction time is 5-9 h; and 2, after the reaction is finished, cooling to 50 DEG C, adding the mixed solvent into a reaction kettle, filtering out the catalyst, cooling the filtrate to 0-3 DEG C, crystallizing,filtering and drying to obtain the white powdery solid N, N-di (beta-ethoxyl) benzamide product. The separation and purification process for synthesizing the N, N-di (beta-ethoxyl) benzamide is simple; the reaction time is moderate, the product yield is high, the product yield reaches 95% or above, the product purity is high, the energy consumption is low, the environmental pollution is small, thecost is low, and the method is an ideal process for realizing industrial production.
High-load, oligomeric phosphonyl dichloride: facile generation via ROM polymerization and application to scavenging amines
Herpel, Russell H.,Vedantham, Punitha,Flynn, Daniel L.,Hanson, Paul R.
, p. 6429 - 6432 (2007/10/03)
A new ROMP-derived scavenging reagent, oligomeric phosphonyl dichloride (OPC), with high-load and selectivity is reported. This reagent can be readily generated via the ROM polymerization of bicyclo[2.2.1]hept-5-en-2-ylphosphonic dichloride, which is conveniently assembled from the Diels-Alder reaction of cyclopentadiene and vinyl phosphonic dichloride. The OPC has been exploited in the rapid, efficient scavenging of primary and secondary amines that are present in excess following a common benzoylation event at room temperature (30-60 min) or under microwave conditions in shorter duration (5 min).