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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2243716Generated: November 2, 2026

Chloroform → HCID 59208144, compound

https://huagongshe.com/reaction/2243716

Reaction equation

Participants

RoleNameHCIDCharge
ReactantChloroformHCID 6212—
ReactantDiisopropylethylamineHCID 81531—
Reactant3-(Dimethylamino)pyrrolidineHCID 2758519—
Reactant3-[8-(2,6-difluorophenyl)-2-(methylsulfinyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-(1-methylethyl)benzamideHCID 11950820—
SolventTetrahydrofuranHCID 8028—
ProductHCID 59208144HCID 5920814476%

Reaction Steps

To a solution of compound 3-[8-(2,6-difluorophenyl)-2-(methylsulfinyl)-7-oxo-5,6,7,8-tetrahydropyrimido[4,5-d]pyrimidin-4-yl]-4-methyl-N-(1-methylethyl)-benzamide (30 mg, 0.06 mmol) in THF (1 mL)/CHCl3 (1 mL) were added N,N-dimethyl-3-pyrrolidinamine (14 mg, 0.12 mmol) and N,N-diisopropylethylamine (0.6 mL, 3.0 mmol). The resultant solution was stirred at room temperature over night. The result mixture was concentrated. CombiFlash chromatography (mobile phase DCM/DCM[90]+MeOH[7]+NH4OH[3]) provided the title compound as a white solid (25 mg, 76%). LC-MS m/z 550 (M+H)+; 1H-NMR (MeOD) δ 1.27 (d, 6H), 1.75 (m, 1H), 2.15 (m, 1H), 2.24 (s, 6H), 2.30 (s, 3H), 2.79 (m, 1H), 3.15 (m, 2H), 3.45 (m, 1H), 3.71 (m, 1H), 4.11 (s, 2H), 4.23 (m, 1H), 7.16 (t, 2H), 7.46 (d, 1H), 7.50 (m, 1H), 7.70 (s, 1H), 7.85 (d, 1H).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS07674789B2
Source datasetuspto-grants-2010_03
ORD IDord-a716c175f36c4870833650f95f280b96
Source noteuspto-grants-2010_03