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HRID 526521作成日:2026年10月26日

1,2-Dichloroethane → HCID 178433410、化合物

https://huagongshe.com/reaction/526521

反応式

関与物質

役割名称HCID仕込み量
反応物1,2-DichloroethaneHCID 11—
反応物1-HydroxybenzotriazoleHCID 75771—
反応物DiisopropylethylamineHCID 81531—
反応物(1-Methylcyclopropyl)amine hydrochlorideHCID 12953687—
反応物HCID 178509615HCID 178509615—
溶媒Dimethyl SulfoxideHCID 679—
溶媒DimethylformamideHCID 6228—
生成物HCID 178433410HCID 17843341051.1%

反応手順

Combined EDC (56.3 mg, 0.294 mmol), HOBT (39.7 mg, 0.294 mmol) and 6-(4-(4-cyanophenyl)-5-hydroxy-1H-pyrazol-1-yl)nicotinic acid (45 mg, 0.147 mmol) in DMF (0.8 mL) then added 1-methylcyclopropanamine hydrochloride (47.4 mg, 0.441 mmol) and Hunig's base (0.180 mL, 1.028 mmol) and stirred at 20° C. for 16 h. The reaction mixture was diluted with 100 uL DMSO and purified by prep HPLC (ACN/water with formic acid) to give the title compound (27 mg, 51.1% yield) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ ppm 0.60-0.68 (m, 2H) 0.73-0.81 (m, 2H) 1.40 (s, 3H) 7.75 (d, J=8.6 Hz, 2H) 8.06-8.16 (m, 2H) 8.35 (dd, J=8.6, 2.3 Hz, 1H) 8.46 (d, J=8.8 Hz, 1H) 8.54 (s, 1H) 8.82-8.90 (m, 2H) 13.53 (br. s., 1H). MS m/z 360 [M+H]+.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09345713B2
出典データセットuspto-grants-2016_05
ORD IDord-774d601518e4466b9c6435e0015ddb94
出典メモuspto-grants-2016_05