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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1259791Generated: November 3, 2026

Water → HCID 59263468, compound

https://huagongshe.com/reaction/1259791

Reaction equation

Participants

RoleNameHCIDCharge
ReactantWaterHCID 962—
Reactant2-BromopyridineHCID 7973—
Reactant1,8-Diazabicyclo(5.4.0)undec-7-eneHCID 81184—
ReactantHCID 66735536HCID 66735536—
CatalystTetrabutylammonium IodideHCID 67553—
SolventDimethylformamideHCID 6228—
ProductHCID 59263468HCID 5926346827%

Reaction Conditions

Temperature120 °C

Reaction Steps

A mixture of 1′-(piperidin-4-ylmethyl)spiro[furo[2,3-f][1,3]benzodioxole-7,3′-indol]-2′(1′H)-one hydrobromide (0.20 g, 0.44 mmol), 2-bromopyridine (0.16 mL, 0.65 mmol), tetrabutyl ammonium iodide (0.05 g) and DBU (0.16 mL, 1.09 mmol) in DMF (5.00 mL) was heated at 120° C. for 15 hrs. After cooling down to ambient temperature, water (30.0 mL) was added. The above mixture was extracted twice with ethyl acetate (50.0 mL), the combined organic phase was dried over Na2SO4 and filtered. The filtrate was concentrated in vacuo to dryness. The residue was subjected to flash chromatography eluting with 30% ethyl acetate in hexane to give a white solid (0.05 g, 27%): mp 95-97° C.; 1H NMR (300 MHz, CDCl3) δ 8.17 (d, 1H), 7.47 (td, 1H), 7.31 (t, 1H), 7.18 (d, 1H), 7.06 (t, 1H), 6.92 (d, 1H), 6.66 (d, 1H), 6.59 (dd, 1H), 6.52 (s, 1H), 6.12 (s, 1H), 5.91-5.84 (m, 2H), 4.91 (d, 1H), 4.66 (d, 1H), 4.42-4.27 (m, 2H), 3.82-3.53 (m, 2H), 2.85 (t, 2H), 2.22-2.05 (m, 1H), 1.85-1.70 (m, 2H), 1.53-1.35 (m, 2H); 13C NMR (75 MHz, CDCl3) δ 177.9, 158.8, 156.1, 149.0, 147.4, 142.8, 142.5, 138.0, 132.4, 129.1, 124.2, 123.5, 119.5, 112.9, 108.8, 107.7, 103.1, 101.7, 93.8, 80.7, 58.3, 46.0, 45.5, 45.4, 35.2, 29.8, 29.7; MS (ES+) m/z 456 (M+1).

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08466188B2
Source datasetuspto-grants-2013_06
ORD IDord-5fb7f7dfe00446c0866b4e0b13b87e63
Source noteuspto-grants-2013_06