2-Methyl-5-hydroxypyridine → 5-(2-Ethoxyethoxy)-2-methylpyridine

HRID 1086251ノート

反応式

HRID 1086251 の反応式
C[O-].[Na+].[OH:4][C:5]1[CH:6]=[CH:7][C:8]([CH3:11])=[N:9][CH:10]=1.C1(C)C=CC(S(O[CH2:22][CH2:23][O:24][CH2:25][CH3:26])(=O)=O)=CC=1>CO>[CH2:23]([O:24][CH2:25][CH2:26][O:4][C:5]1[CH:6]=[CH:7][C:8]([CH3:11])=[N:9][CH:10]=1)[CH3:22]

参加物

5

反応物 3

HCID 142752-Methyl-5-hydroxypyridineHCID 41253902-Ethoxyethyl 4-methylbenzene-1-sulfonateHCID 10942334Sodium Methoxide

生成物 1

HCID 150671045-(2-Ethoxyethoxy)-2-methylpyridine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒3 回

実験手順

A solution of 994 g (18.4 mmol) of sodium methylate in 20 ml of abs. methanol is added dropwise to a solution of 2 g (18.4 mmol) of 5-hydroxy-2-methylpyridine in 20 ml of abs. methanol. The mixture is stirred for 5 minutes and then a solution of 5.83 g (23.9 mmol) of (2-ethoxy)ethyl p-toluenesulphonate in 15 ml of abs. methanol is added. The mixture is heated under reflux for 72 hours. It is evaporated to dryness, the residue is taken up in ethyl acetate and washed with saturated NaCl solution. Drying over sodium sulphate and evaporation result in 2.1 g (70% of theory) of a pale yellow oil.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 72 hours
  3. customIt is evaporated to dryness
  4. washwashed with saturated NaCl solution
  5. dry with materialDrying over sodium sulphate and evaporation
  6. customresult in 2.1 g (70% of theory) of a pale yellow oil

出典と根拠

ORDレコード
ord-545ee36447694178afb9c550dbce3440
出典データセット
uspto-grants-1991_07
特許番号
US05028617

反応ノート

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