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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 919610Generated: October 31, 2026

Methanol → HCID 56968328, compound

https://huagongshe.com/reaction/919610

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethanolHCID 887—
ReactantPotassium CarbonateHCID 11430—
ReactantHCID 118890590HCID 118890590—
SolventDichloromethaneHCID 6344—
SolventMethanol--water (1/1)HCID 22242641—
ProductHCID 56968328HCID 5696832846.2%

Reaction Conditions

Temperature90 °C

Reaction Steps

To a solution of 2-(3,5-dichloro-phenylamino)-1-(3-{methyl-[7-(tosyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-amino}-azepan-1-yl)-ethanone (235 mg. 0.39 mmol) in MeOH:H2O (4:1, 5 mL) was added K2CO3 (216 mg, 1.56 mmol) and heated at 90° C. for 1 h. The reaction mixture was cooled to rt and concentrated in vacuo to give a residue which was subjected to column chromatography (silica gel, gradient MeOH in CH2Cl2) to afford the titled compound (80.6 mg, 46%). 1H NMR (DMSO-d6, 400 MHz): 11.60 (1s, 1H), 8.08 (s, 1H), 7.12 (d, J=4 Hz, 1H), 6.72 (s, 1H), 6.69 (s, 1H), 6.63 (s, 1H), 6.62 (s, 1H), 6.38-6.35 (m, 1H), 4.98-4.85 (m, 1H), 4.29 and 1.28 (2d, J=2.1 Hz, 1H), 4.10-3.88 (m, 3H), 3.65-2.32 (m, 2H), 3.17 (s, 3H), 1.93-1.76 (m, 6H). LC-MS: m/z [M+1]=447.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS09273028B2
Source datasetuspto-grants-2016_03
ORD IDord-d3a3c7c8db12425b9b92ec2d28aea943
Source noteuspto-grants-2016_03