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Methanol → HCID 86343533、化合物

HRID 2202424
ノート
印刷プレビュー

反応式

HRID 2202424 の反応式
[NH2:1][C:2]1[C:7]([CH3:8])=[CH:6][N:5]=[C:4]([Cl:9])[CH:3]=1.[OH:10][C:11]1[CH:16]=[C:15]([CH3:17])[O:14][C:13](=O)[CH:12]=1.[Cl-].[Li+].CO>ClCCl>[Cl:9][C:4]1[CH:3]=[C:2]([N:1]2[C:15]([CH3:17])=[CH:16][C:11]([OH:10])=[CH:12][C:13]2=[O:14])[C:7]([CH3:8])=[CH:6][N:5]=1
参加物反応条件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 887MethanolHCID 433294Lithium ChlorideHCID 126437062-Chloro-5-methylpyridin-4-amineHCID 546757574-Hydroxy-6-methyl-2-pyrone

生成物 1

HCID 86343533HCID 86343533、化合物収率 6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
160 °C

実験手順

A well-powdered mixture of 4-amino-5-methyl-2-chloropyridine (0.5 g, 3.5 mmol), 4-hydroxy-6-methyl-pyrone (0.665 g, 5.3 mmol), and lithium chloride (0.025 g, 0.6 mmol) was heated at 160° C. for 20 min in a sealed tube. The resulting melt was cooled and the product was isolated by silica gel flash chromatography using 3% methanol in dichloromethane. Appropriate fractions were combined, concentrated under reduced pressure and the resulting solid was triturated with ethyl acetate, cooled and filtered. The solid was washed with ethyl acetate and dried to give 0.053 g of the title compound as a yellow powder. ES-MS: m/z=251 (M+H).

後処理

  1. temperatureThe resulting melt was cooled
  2. customthe product was isolated by silica gel flash chromatography
  3. concentrationconcentrated under reduced pressure
  4. customthe resulting solid was triturated with ethyl acetate
  5. temperaturecooled
  6. filtrationfiltered
  7. washThe solid was washed with ethyl acetate
  8. customdried

出典と根拠

ORDレコード
ord-9a19c991c2d04def811a6e29ca1c475a
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09365547B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート