Sulfuric Acid → 2-[5-(2,6-Dimethoxyphenyl)-1-[4-[N-methyl-N-(3-dimethylaminopropyl)carbamoyl]-2-isopropylphenyl]-3-pyrazolylcarbonylamino]-2-adamantanecarboxylic acid hydrogen sulphate

Participants

Role	Name	HCID	Charge
Reactant	Sulfuric Acid	HCID 1118	—
Reactant	Diethyl Ether	HCID 3283	—
Reactant	SR142948A	HCID 5311451	—
Solvent	Methanol	HCID 887	—
Product	2-[5-(2,6-Dimethoxyphenyl)-1-[4-[N-methyl-N-(3-dimethylaminopropyl)carbamoyl]-2-isopropylphenyl]-3-pyrazolylcarbonylamino]-2-adamantanecarboxylic acid hydrogen sulphate	HCID 70246179	94.5%

Reaction Conditions

Temperature	5 °C

Reaction Steps

0.5 g of the compound obtained in EXAMPLE 1' is added to a solution of 0.08 g of H2SO4 in 5 ml of MeOH, this solution is poured into 150 ml of ether cooled to 5° C., and the precipitate formed is drained. 0.54 g of the expected product is obtained. After recrystallization in water, m.p.=212° C. (dec.). After recrystallization in 2-isopropanol, m.p.=263° C.

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US05925661
Source dataset	uspto-grants-1999_07
ORD ID	ord-6743dd7029a74400a67f9515d89c49fc
Source note	uspto-grants-1999_07