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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1951277Generated: November 3, 2026

Trifluoroacetic acid → HCID 58328161, compound

https://huagongshe.com/reaction/1951277

Reaction equation

Participants

RoleNameHCIDCharge
ReactantTrifluoroacetic acidHCID 6422—
ReactantTriethylamineHCID 8471—
ReactantBenzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphateHCID 151348—
Reactant3-amino-N-cyclopropyl-4-methylbenzamideHCID 11983854—
ReactantHCID 67148960HCID 67148960—
SolventMethanolHCID 887—
SolventWaterHCID 962—
SolventDimethylformamideHCID 6228—
ProductHCID 58328161HCID 58328161—

Reaction Steps

To a solution of 3-amino-N-cyclopropyl-4-methylbenzamide (0.025 g, 0.11 mmol) in anhydrous DMF (0.5 mL), are sequentially added 1-(ethoxycarbonyl)-1H-indole-6-carboxylic acid (0.026 g, 0.11 mmol, prepared according to a similar procedure outlined for step A, Example 128 in WO 2002/014308) triethylamine (61 μL, 0.44 mmol) and BOP (0.098 g, 0.22 mmol) at room temperature. The reaction mixture was stirred at room temperature for 18 h, diluted with MeOH (0.5 mL) and subjected to reverse phase preparative HPLC (YMC S5 20×100 mm, 10 min. run, solvent A: 10% MeOH: 90% H2O: 0.1% TFA, solvent B: 90% MeOH, 10% H2O, 0.1% TFA). The desired fractions were collected, and concentrated using speedVac® Plus (SC250DDA) to yield the title compound (Example 218, 0.010 g). HPLC Ret. time (YMC S5 Combiscreen ODS; 4.6×50 mm (4 min. gradient); Solvent A=10% MeOH, 90% H2O, 0.2% H3PO4; solvent B=90% MeOH, 10% H2O, 0.2% H3PO4): 3.18 min. LCMS [M+H]+ 406.3.

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08404689B2
Source datasetuspto-grants-2013_03
ORD IDord-cfe42622e1434649966352fbca8618d7
Source noteuspto-grants-2013_03