2,2,2-Trifluoroethyl trichloromethanesulphonate → HCID 66614606, compound

Participants

Role	Name	HCID	Charge
Reactant	2,2,2-Trifluoroethyl trichloromethanesulphonate	HCID 90027	—
Reactant	2-((1,1-Dimethylethyl)imino)-N,N-diethylhexahydro-1,3-dimethyl-2lambda5-1,3,2-diazaphosphorin-2-amine	HCID 3513851	—
Reactant	6-amino-2-(1-(2-fluorobenzyl)-1H-pyrazolo[3,4-b]pyridin-3-yl)- 7,9-dihydro-8H-purin-8-one	HCID 66613627	—
Solvent	Dimethylformamide	HCID 6228	—
Product	HCID 66614606	HCID 66614606	49.2%

Reaction Conditions

Temperature	0 °C

Reaction Steps

100 mg (0.266 mmol) of the compound from example 33 and 73 mg (0.266 mmol) of BEMP were initially charged in 9 ml of dimethylformamide, and a solution of 75 mg (0.266 mmol) of 2,2,2-trifluoroethyl trichloromethanesulfonate in 1 ml of dimethylformamide was added dropwise at 0° C. within 10 min. The mixture was stirred at 0° C. for 20 min. Subsequently, the reaction solution was concentrated under reduced pressure and the residue was purified by means of preparative HPLC (eluent: methanol/water, gradient 30:70→90:10). 60 mg of the title compound were obtained (47% of theory).

Provenance & Evidence

DOI	10.6084/m9.figshare.5104873.v1
Patent number	US09096592B2
Source dataset	uspto-grants-2015_08
ORD ID	ord-59365c59325c481da489aba023d0cda3
Source note	uspto-grants-2015_08