Cesium carbonate → 2-Methyl-5-(2-methyl-4-nitrophenoxy)pyridine

HRID 877094

反応式

HRID 877094 の反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH3:11].[CH3:12][C:13]1[N:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[CH3:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[O:19][C:16]1[CH:15]=[CH:14][C:13]([CH3:12])=[N:18][CH:17]=1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 142752-Methyl-5-hydroxypyridineHCID 83315Benzene, 1-chloro-2-methyl-4-nitro-

生成物 1

HCID 179901022-Methyl-5-(2-methyl-4-nitrophenoxy)pyridine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

The mixture of 1-chloro-2-methyl-4-nitrobenzene (17.2 g), 6-methylpyridin-3-ol (12 g) and Cs2CO3 (39 g) in DMF (150 mL) was heated at 110° C. for 4 h. The solid was filtered and water (100 mL) and EtOAc (200 mL) were added. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated. The obtained yellow solid was used for the next step directly.

後処理

  1. filtrationThe solid was filtered
  2. additionwater (100 mL) and EtOAc (200 mL) were added
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-33ca47bf8b6d4e3fa5d1d616b29da37c
出典データセット
uspto-grants-2015_03
特許番号
US08987284B2

関連ノート

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