Water → 7-Fluoro-1,5-naphthyridin-2(1H)-one

HRID 385615ノート

反応式

HRID 385615 の反応式
[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][CH:8]=[N+:9]2[O-])=[N:4][CH:3]=1.C1(C)C=CC(S(Cl)(=O)=[O:20])=CC=1.C(=O)([O-])[O-].[K+].[K+].O>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[CH:7][C:8](=[O:20])[NH:9]2)=[N:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 11430Potassium CarbonateHCID 57815215HCID 57815215、化合物

生成物 1

HCID 469008017-Fluoro-1,5-naphthyridin-2(1H)-one収率 23.3%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 60 mg of 7-fluoro-1,5-naphthyridine 1-oxide in 1.6 mL of chloroform, 84 mg of p-toluenesulfonyl chloride, 171 mg of potassium carbonate and 0.5 mL of water were added, and the mixture was stirred at room temperature overnight. The solid was filtered off, and purified by silica gel column chromatography using silica gel; Chromatorex-NH made by Fuji Silysia Chemical Ltd., and an eluent of chloroform:methanol=10:1 to obtain 14 mg of 7-fluoro-1,5-naphthyridin-2(1H)-one as a white solid.

後処理

  1. filtrationThe solid was filtered off
  2. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-5c1595f7189c402b97c6edf44dc6b9d1
出典データセット
uspto-grants-2013_02
特許番号
US08367831B2

反応ノート

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