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Methyl iodide → 4-methoxy-3-[3-[3-(2-hydroxyethoxy)phenyl]-1-oxo-2-propenyl]-1,6-dimethyl-2(1H)-pyridinone

HRID 1669370
ノート
印刷プレビュー

反応式

HRID 1669370 の反応式
[OH:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]([CH3:9])[C:4](=[O:10])[C:3]=1[C:11](=[O:24])[CH:12]=[CH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH2:21][CH2:22][OH:23])[CH:15]=1.[H-].[Na+].I[CH3:28].S([O-])(O)(=O)=O.[Na+]>CN(C)C=O>[CH3:28][O:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]([CH3:9])[C:4](=[O:10])[C:3]=1[C:11](=[O:24])[CH:12]=[CH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([O:20][CH2:21][CH2:22][OH:23])[CH:15]=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 6328Methyl iodideHCID 24758Sodium hydrideHCID 516919Sodium BisulfateHCID 1363442474-hydroxy-3-[3-[3-(2-hydroxyethoxy)phenyl]-1-oxo-2-propenyl]-1,6-dimethyl-2(1H)-pyridinone

生成物 1

HCID 673472144-methoxy-3-[3-[3-(2-hydroxyethoxy)phenyl]-1-oxo-2-propenyl]-1,6-dimethyl-2(1H)-pyridinone収率 45.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a mixture of 1.41 g of 4-hydroxy-3-[3-[3-(2-hydroxyethoxy)phenyl]-1-oxo-2-propenyl]-1,6-dimethyl-2(1H)-pyridinone and 14 ml of dimethylformamide was added 0.19 g of sodium hydride (60% oily) under ice-cooling. After stirred at room temperature for 1 hour, 1.82 g of iodomethane was added, and this was stirred at room temperature to 42° C. for 5 hours. The reaction solution was neutralized with sodium hydrogen sulfate under ice-cooling, this was concentrated under reduced pressure, and the resulting residue was subjected to silica gel column chromatography to obtain 0.67 g of 4-methoxy-3-[3-[3-(2-hydroxyethoxy)phenyl]-1-oxo-2-propenyl]-1,6-dimethyl-2(1H)-pyridinone [Compound No. (41a)] as a yellow crystal.

後処理

  1. temperaturecooling
  2. stirringthis was stirred at room temperature to 42° C. for 5 hours
  3. temperaturecooling
  4. concentrationthis was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-df8400fdff49433097013c0cab41eaad
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07989478B2

反応ノート

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