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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 45010Generated: October 28, 2026

Acetonitrile--water (1/1) → HCID 178509203, compound

https://huagongshe.com/reaction/45010

Reaction equation

Participants

RoleNameHCIDCharge
ReactantAcetonitrile--water (1/1)HCID 18373917—
ReactantHCID 178504222HCID 178504222—
SolventTrifluoroacetic acidHCID 6422—
ProductHCID 178509203HCID 178509203—

Reaction Steps

5-[(cis-4-[4-(7-[2-(Trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]cyclohexylmethyl)thio]-4H-1,2,4-triazol-3-amine (9a) was dissolved in TFA (1 mL) and was stirred for 2 h. The solution was concentrated using a rotary evaporator to remove TFA. The residue was dissolved in methanol (1 mL) and ammonium hydroxide (1 mL) added. The solution was stirred overnight. LCMS showed complete de-protection. The solution was concentrated using a rotary evaporator. The product was isolated by prep LCMS using a 30 mm×100 mm C18 column; 11% CH3CN—H2O (0.1% TFA), 1.5 min, to 33% at 6 min; 60 mL/min; detector set at m/z 396; retention time, 5.5 min (2 runs). The eluate was freeze dried. Yield 21 mg (di-TFA salt). LC/MS (M+H)+: 396,

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08541425B2
Source datasetuspto-grants-2013_09
ORD IDord-761844b4dd914257aad3b42e2c4d41d4
Source noteuspto-grants-2013_09