Methanesulfonic Acid → N-(3-{8-(2,6-difluorophenyl)-7-oxo-2-[(2,2,6,6-tetramethyl-4-piperidinyl)amino]-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl}-4-methylphenyl)-3-thiophenecarboxamide methanesulfonate

Participants

Role	Name	HCID	Charge
Reactant	Methanesulfonic Acid	HCID 6395	—
Reactant	N-(3-{8-(2,6-difluorophenyl)-7-oxo-2-[(2,2,6,6-tetramethyl-4-piperidinyl)amino]-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl]-4-methylphenyl)-3-thiophenecarboxamide	HCID 11947981	—
Solvent	Acetonitrile	HCID 6342	—
Product	N-(3-{8-(2,6-difluorophenyl)-7-oxo-2-[(2,2,6,6-tetramethyl-4-piperidinyl)amino]-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl}-4-methylphenyl)-3-thiophenecarboxamide methanesulfonate	HCID 86608569	—

Reaction Conditions

Temperature	60 °C

Reaction Steps

Added 320 uL of CH3CN to N-(3-{8-(2,6-difluorophenyl)-7-oxo-2-[(2,2,6,6-tetramethyl-4-piperidinyl)amino]-7,8-dihydropyrido[2,3-d]pyrimidin-4-yl}-4-methylphenyl)-3-thiophenecarboxamide (16.0 mg) and heated to about 60° C. Added methanesulfonic acid (1.1 eq; 1M in IPA), and solution clarified except for tiny amount stuck to bottom. After a few minutes at about 60° C., cooled to rt. Got lots of white precipitate. Stirred overnight at rt. Next day, filtered and dried to provide the title compound (3.5 mg). Melting point (tested with DSC) is 331° C.

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US08207176B2
Source dataset	uspto-grants-2012_06
ORD ID	ord-b48633af8382447b8437712ef4ed1ccc
Source note	uspto-grants-2012_06