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HRID 80895作成日:2026年10月24日

Potassium Carbonate → HCID 131730771、化合物

https://huagongshe.com/ja/reaction/80895

反応式

関与物質

役割名称HCID仕込み量
反応物Potassium CarbonateHCID 11430—
反応物Pyridazine, 3-chloro-6-[4-(trifluoromethyl)phenyl]-HCID 12449554—
反応物Piperidin-3-amine dihydrochlorideHCID 16211870—
溶媒AcetoneHCID 180—
生成物HCID 131730771HCID 13173077127.5%

反応条件

温度120 °C

反応手順

3-Chloro-6-(4-trifluoromethylphenyl)pyridazine (0.2 g, 0.77 mmol), 3-aminopiperidine dihydrochloride (0.27 g, 1.54 mmol) and potassium carbonate (0.53 g, 3.87 mmol) were mixed in acetone (4 mL) in a 20 mL microwave vessel. The reaction mixture was heated in a microwave oven for 2 h at 120° C. The reaction mixture was filtered and the precipitate was washed with MeOH. The combined organic phases were evaporated. The crude oil was purified on a silicagel column (0.04-0.063 mesh) using dichloromethane/MeOH (9:1) as eluent. This afforded 110 mg of a oil that was dissolved in MeOH and acidified with concentrated HCl (5 mL). The mixture was evaporated and the residue was dissolved in MeOH (1 mL) and ether (100 mL) was added with stirring. The mixture was evaporated to give 76 mg (25%) of the title compound as a yellow solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08846677B2
出典データセットuspto-grants-2014_09
ORD IDord-fee32dfc11fb4f769ef6a6273104e86b
出典メモuspto-grants-2014_09