ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
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
  1. ホーム
  2. /反応

Water → 1-biphenyl-3-yl-5-[(4-methoxybenzyl)oxy]-2-methylpyridin-4(1H)-one

HRID 1056900
ノート
印刷プレビュー

反応式

HRID 1056900 の反応式
[C:1]1([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:6]=[CH:5][CH:4]=[C:3]([N:7]2[CH:12]=[C:11]([OH:13])[C:10](=[O:14])[CH:9]=[C:8]2[CH3:15])[CH:2]=1.[CH3:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([CH2:30]Cl)=[CH:26][CH:25]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[C:1]1([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:6]=[CH:5][CH:4]=[C:3]([N:7]2[CH:12]=[C:11]([O:13][CH2:30][C:27]3[CH:28]=[CH:29][C:24]([O:23][CH3:22])=[CH:25][CH:26]=3)[C:10](=[O:14])[CH:9]=[C:8]2[CH3:15])[CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 699934-Methyloxybenzyl chlorideHCID 674185551-biphenyl-3-yl-5-hydroxy-2-methylpyridin-4(1H)-one

生成物 1

HCID 674181761-biphenyl-3-yl-5-[(4-methoxybenzyl)oxy]-2-methylpyridin-4(1H)-one

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 4.8 g (17.4 mmol) l-biphenyl-3-yl-5-hydroxy-2-methylpyridin-4(1H)-one in 150 ml of DMF was added 4.1 g (26.1 mmol) PMBCl, and 12.0 g (87.0 mmol) K2CO3. The reaction was stirred at rt for 2 h, after which time water was added and a precipitate formed. The solid was collected by filtration and purified by flash chromatography (100 g silica gel, 0-20% MeOH;EtOAc) to afford 1-biphenyl-3-yl-5-[(4-methoxybenzyl)oxy]-2-methylpyridin-4(1H)-one.  H NM δ (ppm)(DMSO-d6): 7.84 (1H, d, J=7.86 Hz), 7.77 (2H, d, J=7.71 Hz), 7.73 (1H, s), 7.64 (1H, t, J=7.84 Hz), 7.53-7.47 (3H, m), 7.46-7.39 (2H, m), 7.38-7.30 (3H, m), 6.93 (2H, d, J=8.32 Hz), 6.23 (1H, s), 4.89 (2H, s), 3.77-3.70 (3H, m), 2.03 (3H, s). LCMS (M+H)+=398.3.

後処理

  1. customa precipitate formed
  2. filtrationThe solid was collected by filtration
  3. custompurified by flash chromatography (100 g silica gel, 0-20% MeOH;EtOAc)

出典と根拠

ORDレコード
ord-ce16ba1d3afc4072961f5d71cd05c048
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09399651B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート