反应详情

Into the same reactor as used in the previous step were poured 30 g (0.1 mol) of bis (isopropylguanidine) sulphate, 120 ml of water, 75 ml of pure hydrochloric acid solution (s.g. 1.18) and slowly (over 11/2 hours), at room temperature, 44 g (0.2 mol) of 1,1,3,3-tetraethoxy propane. The mixture was then heated to 50°-55° C. under stirring for two hours, then cooled and neutralized by an excess of pure sodium hydroxide solution. The mixture was extracted using 300 ml of diethyl ether. The extracts were washed with a saturated solution of sodium chloride, then dried and the diethyl ether was evacuated off. There was obtained 25 g (yield 91%) of a yellowish oil boiling at 91°-91.5° C. under 11 mm of Hg, the analysis of which showed good correspondence with the formula C7H11N3.

1. customat room temperature
2. temperatureThe mixture was then heated to 50°-55° C.
3. temperaturecooled
4. extractionThe mixture was extracted
5. washThe extracts were washed with a saturated solution of sodium chloride
6. customdried
7. customthe diethyl ether was evacuated off