反应详情

温度

75 °C

A mixture of 5.69 grams (20 mmol) of tetra-n-butylurea, 3.22 grams (21 mmol) of phosphorus oxychloride and 15 ml of acetonitrile was heated at 75° C. in a nitrogen atmosphere for one hour. The mixture was then cooled to 0° C. and 3.36 grams (46 mmol) of n-butylamine was added over 15 minutes with stirring. The mixture was warmed to 60° C. for one hour and again cooled to 0° C., quenched with 5 ml of 25% (by weight) aqueous sodium hydroxide solution and extracted with diethylether. The ether extracts were dried over sodium sulphate, filtered and stripped to give a pale yellow oil of penta-n-butylguanidine.

1. temperatureThe mixture was then cooled to 0° C.
2. temperatureThe mixture was warmed to 60° C. for one hour
3. temperatureagain cooled to 0° C.
4. customquenched with 5 ml of 25% (by weight) aqueous sodium hydroxide solution
5. extractionextracted with diethylether
6. dry with materialThe ether extracts were dried over sodium sulphate
7. filtrationfiltered