N-butylbutan-1-amine;hydrochloride

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 200 g of methyl methacrylate, 129 g of dibutylamine, 8.25 g of dibutylamine hydrochloride, 5 g of Fe-(III)-acetylacetonate, and 0.5 g of hydroquinone were heated for 3 hours at 230° C. in an autoclave (pmax =10 atmospheres). In this way, a 15% yield of N,N-dibutylmethacrylic acid amide form. The selectivity, calculated on the methyl methacrylate reacted, was greater than 80%.

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Tolylene diisocyanate (2,4-tolylene diisocyanate/2,6-tolylene diisocyanate=80/20, hereinafter referred to as "TDI", 174 g) and EGA (130 g) are mixed, and to the stirred mixture is added dropwise HEMA (130 g, wherein phenothiazine (0.13 g) is dissolved) under nitrogen gas at 20°-45° C. over a period of 1 hour. After finishing the dropping of HEMA, the mixture is heated to 60° C. in 30 minutes and is stirred at the same temperature for 1.5 hour. It is confirmed that the product contains NCO of 9.6% (measured by di-n-butylamine-hydrochloric acid titration method) and an isocyanate product semi-blocked with HEMA is produced. are mixed

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Tolylene diisocyanate (2,4-tolylene diisocyanate/2,6-tolylene diisocyanate=80/20, hereinafter referred to as "TDI", 174 g) and EGA (130 g) are mixed, and to the stirred mixture is added dropwise HEMA (130 g, wherein phenothiazine (0.13 g) is dissolved) under nitrogen gas at 20°-45° C. over a period of 1 hour. After finishing the dropping of HEMA, the mixture is heated to 60° C. in 30 minutes and is stirred at the same temperature for 1.5 hour. It is confirmed that the product contains NCO of 9.6% (measured by di-n-butylamine-hydrochloric acid titration method) and an isocyanate product semi-blocked with HEMA is produced. are mixed

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A solution of 68.7 g (0.5 mole) of phosphorus trichloride in dry hexane or diethyl ether is added slowly to a stirred solution of 363.6 g (3.0 moles) of dibutylamine in the same solvent. A voluminous precipitate of dibutylamine hydrochloride is formed, the temperature remaining between 10° and 40° C. After all the phosphorus trichloride has been added, the mixture is boiled and refluxed for between 30 minutes and 2 hours. The mixture is then cooled to room temperature and filtered to separate it from 280 g (1.7 moles) of dibutylamine hydrochloride. The solvent is then stripped off at reduced pressure in a rotary evaporator.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 200 g of methyl methacrylate, 129 g of dibutylamine, 8.25 g of dibutylamine hydrochloride, 5 g of Fe-(III)-acetylacetonate, and 0.5 g of hydroquinone were heated for 3 hours at 230° C. in an autoclave (pmax =10 atmospheres). In this way, a 15% yield of N,N-dibutylmethacrylic acid amide form. The selectivity, calculated on the methyl methacrylate reacted, was greater than 80%.

Conditions: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Tolylene diisocyanate (2,4-tolylene diisocyanate/2,6-tolylene diisocyanate=80/20, hereinafter referred to as "TDI", 174 g) and EGA (130 g) are mixed, and to the stirred mixture is added dropwise HEMA (130 g, wherein phenothiazine (0.13 g) is dissolved) under nitrogen gas at 20°-45° C. over a period of 1 hour. After finishing the dropping of HEMA, the mixture is heated to 60° C. in 30 minutes and is stirred at the same temperature for 1.5 hour. It is confirmed that the product contains NCO of 9.6% (measured by di-n-butylamine-hydrochloric acid titration method) and an isocyanate product semi-blocked with HEMA is produced. are mixed