反应详情

A mixture of 1-chloro-3-(dimethylamino)-2-methylpropane hydrochloride (200 g), thiourea (97.3 g) and ethanol (950 ml) was stirred and heated under reflux for 72 hours. The solution was allowed to cool and the solvent was removed in vacuo. The residue was dissolved in a small volume of ethanol and ether was added until the first permanent opalescence was observed. The mixture was stored at 4° C. for 16 hours. The solvent was removed in yacuo to afford a waxy/oily solid which was dried in vacuo over calcium chloride for 48 hours, then triturated with propan-2-ol. The resulting solid was collected by filtration, washed with propan-2-ol, and dried in vacuo to give S-[3-(dimethylamino)-2-methylpropyl]isothiourea dihydrochloride as a pale brown solid (90 g).

1. temperatureheated
2. temperatureunder reflux for 72 hours
3. temperatureto cool
4. customthe solvent was removed in vacuo
5. dissolutionThe residue was dissolved in a small volume of ethanol and ether
6. additionwas added until the first permanent opalescence
7. customThe solvent was removed in yacuo
8. customto afford a waxy/oily solid which
9. dry with materialwas dried in vacuo over calcium chloride for 48 hours
10. customtriturated with propan-2-ol
11. filtrationThe resulting solid was collected by filtration
12. washwashed with propan-2-ol
13. customdried in vacuo