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HRID 78563作成日:2026年10月25日

Methane → HCID 52937760、化合物

https://huagongshe.com/reaction/78563

反応式

関与物質

役割名称HCID仕込み量
反応物MethaneHCID 297—
反応物O-PhenylenediamineHCID 7243—
反応物TriethylamineHCID 8471—
反応物Diethyl cyanophosphonateHCID 76257—
反応物3-Amino-6-bromopyrazine-2-carboxylic acidHCID 18521600—
溶媒WaterHCID 962—
溶媒1,2-DimethoxyethaneHCID 8071—
溶媒Ethyl AcetateHCID 8857—
生成物HCID 52937760HCID 5293776060.4%

反応条件

温度170 °C

反応手順

A mixture of 3-amino-6-bromo-pyrazine-2-carboxylic acid (10 g, 45.87 mmol), benzene-1,2-diamine (5.45 g, 50.46 mmol), diethoxyphosphorylformonitrile (8.23 g, 50.46 mmol) and triethylamine (12.79 mL, 91.74 mmol) in DME (30 mL) was heated in the microwave at 170° C. for 40 minutes. The mixture was allowed to cool and water was added. The resultant dark-coloured precipitate was dissolved in EtOAc and stirred with charcoal for 30 minutes. After filtering through celite, the filtrate was concentrated in vacuo to give the product as a yellow solid (8.04 g, 60% Yield). 1H NMR (400 MHz, DMSO) 7.22-7.32 (2H, m), 7.55 (1H, d), 7.75 (1H, d), 7.8 (1 h, br s), 8.8 (1H, br s), 13.1 (1H, s); MS (ES+) 291

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08841308B2
出典データセットuspto-grants-2014_09
ORD IDord-3098fade2ad445e28fe562e67f568c00
出典メモuspto-grants-2014_09