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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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2-Chloro-5-nitroisonicotinaldehyde → 1-(2-Chloro-5-nitropyridin-4-yl)ethan-1-one

HRID 1028040
ノート
印刷プレビュー

反応式

HRID 1028040 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:7]([N+:10]([O-:12])=[O:11])=[CH:8][N:9]=1)[CH:5]=[O:6].[CH3:13][Li]>[Ti](Cl)(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[C:4]([C:5](=[O:6])[CH3:13])[C:7]([N+:10]([O-:12])=[O:11])=[CH:8][N:9]=1
参加物実験手順出典と根拠反応ノート

参加物

4

反応物 2

HCID 469162492-Chloro-5-nitroisonicotinaldehydeHCID 178418348HCID 178418348、化合物

生成物 1

HCID 583875681-(2-Chloro-5-nitropyridin-4-yl)ethan-1-one

試薬・触媒・溶媒 1

HCID 24193Titanium Tetrachloride触媒

実験手順

A route to prepare 4-hydroxy 6-chloro 1,7 napthyridine is depicted in Scheme III. Starting with 2-chloro-4-methyl-5-nitropyridine, condensation with dimethylformamidedimethylacetal and subsequent oxidative cleavage yields 2-chloro-5-nitroisonicotinaldehyde. Chemoselective methyl addition to the aldehyde with methyllithium and titaniumtetrachloride at −50° C. followed by oxidation yields 1-(2-chloro-5-nitropyridin-4-yl)ethanone. Nitro reduction with iron in acetic acid, followed by a two step monotosylation yields N-(4-acetyl-6-chloropyridin-3-yl)-4-nitrobenzenesulfonamide. Upon heating with dimethylformamidedimethylacetal and diisopropylethylamine in DMF at 105° C. and subsequent treatment with thiophenol at room temperature, 6-chloro-1,7-naphthyridin-4-ol is obtained IV. Conversion of IV to the corresponding triflate or benzyl ether using standard conditions yields bifunctional intermediates which can be taken through the chemical transformation depicted in Schemes 1 and 2 to yield 4,6 disubstituted 1,7 naphthyridines V.

出典と根拠

ORDレコード
ord-3fd27bbf74fe48469777c9fe39abba7e
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735424B2

反応ノート

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