반응 #649754
ord-babd8341accc41f09964f38c2c0f1462
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타When the exothermic reaction
- 2workup.ADDITIONare added
- 3온도at reflux for 25 hours
- 4온도cooled to 0.degree
- 5여과and filtered
- 6세척Washing with 4.times
- 7건조100 ml of ethanol/diethyl ether (1:1) and drying
실험 절차
9.1 ml (0.13 mol) of 65% nitric acid are added dropwise in the course of 5 minutes to a yellow suspension of 20.0 g (0.13 mol) of 2-amino-4-nitrotoluene in 50 ml of absolute ethanol. When the exothermic reaction has subsided, 8.32 g (0.198 mol) of cyanamide dissolved in 8.3 ml of water are added. The brown reaction mixture is boiled at reflux for 25 hours, cooled to 0.degree. and filtered. Washing with 4.times.100 ml of ethanol/diethyl ether (1:1) and drying yield 2-methyl-5-nitrophenyl-guanidine nitrate; m.p. 219° C.-226° C.