関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | 2-Amino-4'-chlorobenzophenone | HCID 76166 | — |
| 反応物 | 2-Chloro-3-pyridylamine | HCID 80528 | — |
| 生成物 | [2-[(3-Amino-2-pyridinyl)amino]-4-chlorophenyl]phenylmethanone | HCID 15586654 | — |
反応手順
A stirred mixture of 23.2 g (0.1 mole) of 2-amino-4'-chlorobenzophenone and 14.2 g (0.11 mole) of 3-amino-2-chloropyridine was heated at 180° C. under nitrogen atmosphere for 2.5 hr. The mixture solidified upon cooling to room temperature and was broken up with a spatula. The solid was suspended in 100 ml of methylene chloride and collected by filtration. The filter cake was dissolved in a mixture of water-methanol, basified with 3N sodium hydroxide and extracted twice with methylene chloride. The combined methylene chloride extracts were dried over magnesium sulfate and evaporated under reduced pressure. The residue which had crystallized was triturated in isopropyl ether and the solid (16.7 g) collected by filtration. A 3 g sample was recrystallized from isopropyl ether to give 1.6 g product;
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04556667 |
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| 出典データセット | uspto-grants-1985_12 |
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| ORD ID | ord-9c83145362884b74b0da654c1bd5c857 |
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| 出典メモ | uspto-grants-1985_12 |
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