dimethyl 2,2-diethylpropanedioate

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

Procedure: After the addition of 1 g of tetrabutyl-orthotitanate, 47 g of dimethyl diethylmalonate and 98.6 g of 1-allyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 100 ml of xylene are heated under a gentle stream of nitrogen to about 140°. The methanol forming during the reaction is continuously distilled off, and after about 6 hours the reaction is virtually completed. The reaction mixture is diluted with 200 ml of toluene, extracted three times with 100 ml of water each time, dried over sodium sulphate and concentrated by evaporation. Crystallisation of the residue from hexane yields bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl) diethylmalonate (compound 18), m.p. 135°-136°. are heated under a gentle stream of nitrogen to about 140° The methanol forming during the reaction is continuously distilled off The reaction mixture is diluted with 200 ml of toluene extracted three times with 100 ml of water each time dried over sodium sulphate concentrated by evaporation Crystallisation of the residue from hexane

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

Procedure: After the addition of 1 g of tetrabutyl-orthotitanate, 47 g of dimethyl diethylmalonate and 98.6 g of 1-allyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 100 ml of xylene are heated under a gentle stream of nitrogen to about 140°. The methanol forming during the reaction is continuously distilled off, and after about 6 hours the reaction is virtually completed. The reaction mixture is diluted with 200 ml of toluene, extracted three times with 100 ml of water each time, dried over sodium sulphate and concentrated by evaporation. Crystallisation of the residue from hexane yields bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl)diethylmalonate (compound 18), m.p. 135°-136°. are heated under a gentle stream of nitrogen to about 140° The methanol forming during the reaction is continuously distilled off The reaction mixture is diluted with 200 ml of toluene extracted three times with 100 ml of water each time dried over sodium sulphate concentrated by evaporation Crystallisation of the residue from hexane

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

Procedure: After the addition of 1 g of tetrabutyl-orthotitanate, 47 g of dimethyl diethylmalonate and 98.6 g of 1-allyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 100 ml of xylene are heated under a gentle stream of nitrogen to about 140°. The methanol forming during the reaction is continuously distilled off, and after about 6 hours the reaction is virtually completed. The reaction mixture is diluted with 200 ml of toluene, extracted three times with 100 ml of water each time, dried over sodium sulphate and concentrated by evaporation. Crystallisation of the residue from hexane yields bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl) diethylmalonate (compound 18), m.p. 135°-136°. are heated under a gentle stream of nitrogen to about 140° The methanol forming during the reaction is continuously distilled off The reaction mixture is diluted with 200 ml of toluene extracted three times with 100 ml of water each time dried over sodium sulphate concentrated by evaporation Crystallisation of the residue from hexane