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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2097097Generated: October 30, 2026

1,2-Dichloroethane → HCID 16660149, compound

https://huagongshe.com/reaction/2097097

Reaction equation

Participants

RoleNameHCIDCharge
Reactant1,2-DichloroethaneHCID 11—
Reactant1-HydroxybenzotriazoleHCID 75771—
ReactantDiisopropylethylamineHCID 81531—
ReactantHCID 66967079HCID 66967079—
ReactantMethyl(2-methylbenzofuran-3-ylmethyl)amineHCID 66967084—
SolventWaterHCID 962—
SolventDimethylformamideHCID 6228—
ProductHCID 16660149HCID 1666014973%

Reaction Steps

EDC (0.13 g, 0.70 mmol) was added to a suspension of (E)-3-[6-Amino-5-(1-hydroxy-1-methyl-ethyl)-pyridin-3-yl]-acrylic acid hydrochloride (0.15 g, 0.58 mmol), HOBt (0.09 g, 0.64 mmol), methyl-(2-methyl-benzofuran-3-ylmethyl)-amine (0.11 g, 0.64 mmol) and (i-Pr)2EtN (0.60 mL, 2.48 mmol) in DMF (6 mL). The mixture was allowed to stir overnight at room temperature. The mixture was cooled to 0° C. and diluted with H2O (15 mL) with rapid stirring. The resulting precipitate was filtered, washed with H2O (20 mL) then dried under high vacuum. The solid was then triturated with Et2O, and the resultant beige solid was collected, to yield 160 mg (73%) of product. 1H NMR (300 MHz, DMSO-d6) δ 8.14 (s, 1H), 7.67-7.47 (m, 4H), 7.26-6.99 (m, 3H), 6.58 (s, 2H), 5.49 (s, 1H), 4.80 and 4.74 (2×s, 2H), 3.04 and 2.85 (2×s, 3H), 2.52 (s, 3H), 1.53 (s, 6H); ESI MS m/z 380 [C22H25N3O3+H]+

Provenance & Evidence

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS08450307B2
Source datasetuspto-grants-2013_05
ORD IDord-238a3b7ab092486b8782a5fe32105a34
Source noteuspto-grants-2013_05