Phosphorus sulfide (P2S5) → (+/-)-5-(7-Chloro-1,2-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]imidazol-4-yl)-1-methyl-3,4-dihydro-4-thioxo-2(1H)-pyrimidinone

Participants

Role	Name	HCID	Charge
Reactant	Phosphorus sulfide (P2S5)	HCID 14817	—
Reactant	(+/-)-5-(7-Chloro-1,2-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]imidazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione	HCID 22003604	—
Solvent	1,4-Dioxane	HCID 31275	—
Product	(+/-)-5-(7-Chloro-1,2-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]imidazol-4-yl)-1-methyl-3,4-dihydro-4-thioxo-2(1H)-pyrimidinone	HCID 9864902	—

Reaction Conditions

Temperature	100 °C

Reaction Steps

A mixture of the product from step (iv) (0.535 g), and phosphorus pentasulphide (0.967 g) in 1,4-dioxane (10 ml) was heated at 100° C. for 3 h. The solvent evaporated and the residue dissolved in dichloromethane, washed with saturated aqueous sodium bicarbonate solution then with water, dried (MgSO4) and evaporated. Purification was by chromatography on a biotage silica column, using 3% methanol/0.1% 0.880 ammonia in dichloromethane as eluant.

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US06218376B1
Source dataset	uspto-grants-2001_04
ORD ID	ord-8d5bc3205c97433d978de526e17fa292
Source note	uspto-grants-2001_04