Methanol → HCID 22341585, compound

Temperature

25 °C

To a solution of dimethylcyanamide (10.0 g, 142.7 mmol) in methanol (50 mL) was added dropwise sulfuric acid (14.0 g, 142.7 mmol) over 2 hours at 20-30° C. The mixture was stirred at 20-30° C. for 4 hours and then concentrated in vacuo. To the residue was added acetone (50 mL) and stirred at 20-30° C. After crystallized, the mixture was stirred at 20-30° C. for 30 minutes, then at 0-10° C. for 1 hour and filtered. The crystals were washed with acetone (20 mL) and dried in vacuo to give N,N,O-trimethylisourea sulfate (22.86 g, 80.0% yield) as white granulated solids.

1. concentrationconcentrated in vacuo
2. additionTo the residue was added acetone (50 mL)
3. stirringstirred at 20-30° C
4. customAfter crystallized
5. stirringthe mixture was stirred at 20-30° C. for 30 minutes
6. waitat 0-10° C. for 1 hour
7. filtrationfiltered
8. washThe crystals were washed with acetone (20 mL)
9. customdried in vacuo

ORD record

ord-034713bb71ad4057b5f1f0cc15573199

Source dataset

uspto-grants-2005_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06927230B2