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(3-morpholino-1,2,5-thiadiazol-4-yloxy)-2,2-dimethyl-1,3-dioxolanyl methane[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
In tert-butyl alcohol;
Step A: <strong>[30165-96-9]3-Morpholino-4-chloro-1,2,5-thiadiazole</strong> (1 g., 5 mmole), 2,2-dimethyl-1,3-dioxolan-4-yl methanol (0.7 g., 5 mmole) were heated under reflux for 2 hours in t-butanol containing potassium t-butoxide (0.7 g.). The reaction mixture was diluted with water (10 ml.) and extracted twice with ethyl acetate. After washing with water and drying over magnesium sulfate, evaporation provided 1.35 g. (90%) of (3-morpholino-1,2,5-thiadiazol-4-yloxy)-2,2-dimethyl-1,3-dioxolanyl methane in the form of a yellow oil.
4-(4-(2,2,5,5-tetramethylpyrrolidin-1-oxyl-3-yloxy)-1,2,5-thiadiazol-3-yl)morpholine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
20%
Step a: Preparation of (4-(4-(2,2,5,5-tetramethylpyrrolidin-l-oxyl-3-yloxy)-l,2,5- thiadiazol-3-yl)morpholine. To a solution of 3-hydroxypyrroline-l-oxyl (0.87g, 5.5 mmol) in t- BuOH(50mL), t-BuOK(0.81g, 7.2 mmol) was added. After the mixture was stirred for half an hour, 4-(4-chloro-l,2,5-thiadiazol-3-yl)morpholine (1.3g, 6.3 mmol) was added. The mixture was stirred at 40 C for 2 days. Then the reaction was quenched by adding 50 mL of water to the reaction mixture. The mixture was extracted with EtOAc( 3 x 150ml). The combined organic phase was washed with brine (50 mL) and was concentrated in vacuum. The crude solid was purified by column chromatography (silica gel, EtOAc/Hexane: 1:5). 0.36 g of orange solid was obtained. The yield was 20%.
20%
To a solution of 3-hydroxypyrroline-1-oxyl (0.87 g, 5.5 mmol) in t-BuOH(50 mL), t-BuOK (0.81 g, 7.2 mmol) was added. After the mixture was stirred for half an hour, <strong>[30165-96-9]4-(4-chloro-1,2,5-thiadiazol-3-yl)morpholine</strong> (1.3 g, 6.3 mmol) was added. The mixture was stirred at 40 C. for 2 days. Then the reaction was quenched by adding 50 mL of water to the reaction mixture. The mixture was extracted with EtOAc (3×150 ml). The combined organic phase was washed with brine (50 mL) and was concentrated in vacuum. The crude solid was purified by column chromatography (silica gel, EtOAc/Hexane: 1:5). 0.36 g of orange solid was obtained. The yield was 20%.
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