Methanimidamide, N,N'-bis[(methylamino)carbonyl]- synthesis
- Product Name:Methanimidamide, N,N'-bis[(methylamino)carbonyl]-
- CAS Number:65906-68-5
- Molecular formula:C5H10N4O2
- Molecular Weight:158.16
Yield:65906-68-5 65%
Reaction Conditions:
at 100; for 10 h;
Steps:
2 Stage 2: Preparation of l-methyl-3-methylcarbamoyliminomethyl urea
A suspension of monomethyl urea (50g, 0.67 mol.) in tri ethyl orthoformate (150 ml, 0.90 mol.) was heated to reflux at 120°C bath temperature and internal temperature 100°C for 10 hrs. Reaction progress checked by HPLC. After reaction completion the reaction mixture was cooled to 5-10°C, and stirred for 1 hour to ensure complete precipitation, of the product. The resulting solid was filtered, washed with ethyl acetate (25 ml) and dried under vacuum at 45-50°C to yield 35 g (65 %) of title compound. Purity (by HPLC): 95.66 %.
References:
WO2020/194168,2020,A1 Location in patent:Page/Page column 15
