Hydrochloric Acid → HCID 316821, compound

Temperature

0 °C

9.14 g (97.11 mmol) of 4-methylpyrimidine was slowly added to a 0° C. solution of 8.75 g HCl in 40 ml EtOH. To this white suspension was added, over 5 min, 61 ml of a 10-20% by weight solution of ethyl nitrite in EtOH. The reaction was stirred at 0° C. for 10 min and then at RT for 2.5 h. The white salt was filtered and dried under vacuum. The salt was dissolved into 20 ml H2O and very slowly treated with about 200 ml saturated aqueous KHCO3. A white solid precipitated out of the purple solution. The solid was filtered and dried under vacuum to yield the titled compound.

1. additionTo this white suspension was added, over 5 min
2. waitat RT for 2.5 h
3. filtrationThe white salt was filtered
4. customdried under vacuum
5. dissolutionThe salt was dissolved into 20 ml H2O
6. additionvery slowly treated with about 200 ml saturated aqueous KHCO3
7. customA white solid precipitated out of the purple solution
8. filtrationThe solid was filtered
9. customdried under vacuum

ORD record

ord-a7e9d0c8acb0496eaffb383fe0370721

Source dataset

uspto-grants-2012_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08247430B2