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Formic acid, 255.7g (ie, 38.3g of water) and 99percent of diisopropylamine, 460g, with a purity of 85percent, are added to a 1-liter autoclave,The stirrer was started to mix well and a homogeneous reaction system was obtained. The molar ratio of formic acid to diisopropylamine is 1.05:1.While maintaining the stirring, the above homogeneous reaction system is heated up to about 200° C., the pressure in the autoclave rises to about 1.7 MPa and no longer increases, the reaction is maintained for about 3 hours, and the autoclave is vented and discharged. The carbon monoxide and water vapor were collected and the reaction product was collected to obtain about 709 g of a uniform and transparent solution.
Reference：
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[12] Patent: CN107501115, 2017, A, . Location in patent: Paragraph 0076-0080
2
[ 124-38-9 ]
[ 108-18-9 ]
[ 2700-30-3 ]
Yield
Reaction Conditions
Operation in experiment
13 %Spectr.
Stage #1: With sodium hydride In N,N-dimethyl-formamide at 20℃; for 0.0833333 h; Sealed tube Stage #2: With diphenylsilane In N,N-dimethyl-formamide at 20℃; for 18 h; Sealed tube
General procedure: 0.05mmol equivalent of poly-imidazolium, an equimolar amount of sodium hydride, and 2mL of anhydrous DMF were placed in a crimp-top vial (8mL). The vial was sealed, and the suspension was stirred for 2h before CO2 was introduced via a balloon. Amines (1mmol) were subsequently added, and the reaction mixture was then allowed to stir for 5min before 2.5 equivalents of silane were added. The reaction was allowed to stir for 18h. After the reaction was completed, the reaction mixture was centrifuged, a 400-μL aliquot was sampled, and 20μL of mesitylene was added. An aliquot was then taken for NMR spectroscopy. For catalyst recycling, the remaining solution was decanted, and 2mL of fresh DMF was added. The reaction was allowed to stir for 30min before centrifuging and removal of DMF. This procedure was repeated at least three times using DMF (1×) and dichloromethane (3×) as the washing solvent. The recovered catalyst was then dried under the Schlenk line, and used directly for the next run.
Reference：
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