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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 919619Generated: October 31, 2026

Water → HCID 67516775, compound

https://huagongshe.com/reaction/919619

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
ReactantPotassium CarbonateHCID 11430—
ReactantHCID 86706478HCID 86706478—
SolventMethanolHCID 887—
SolventEthyl AcetateHCID 8857—
ProductHCID 67516775HCID 6751677527.1%

Reaction Conditions

Temperature60 °C

Reaction Steps

To a solution of 2-(3,5-dichlorophenylamino)-1-(4-methyl-3-(7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylamino)piperidin-1-yl)ethanone (100 mg, 0.17 mmol) in MeOH:H2O (4:1 mL) was added K2CO3 (94 mg, 0.68 mmol) and the reaction mixture was heated to 60° C. for 1 h. The reaction mixture was concentrated in vacuo and the residue obtained was diluted in EtOAc (50 mL). The EtOAc suspension was filtered through celite, the filtrate was dried over Na2SO4, and concentrated in vacuo to give a residue that was subjected to purification by column chromatography (silica gel, gradient MeOH in DCM) to afford the titled intermediate (20 mg, 27%). 1H NMR (400 MHz, DMSO-d6): δ 11.61-11.45 (m, 1H), 8.19-8.06 (m, 1H), 7.08-6.43 (m, 5H), 6.22-6.15 (m, 1H), 4.59-4.21 (m, 2H), 4.15-3.75 (m, 3H), 3.25-2.98 (m, 2H), 2.78-2.45 (m, 1H), 2.15-1.99 (m, 1H), 1.86-1.7-62 (m, 2H), 0.98-0.77 (m, 3H). LC-MS: m/z [M+1]=433.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09273028B2
Source datasetuspto-grants-2016_03
ORD IDord-5e7f282a1b924f9bb8b0cc62d0df86e4
Source noteuspto-grants-2016_03