Sodium hydride → 2-Methoxy-4-methylpyridine

HRID 647984ノート

反応式

HRID 647984 の反応式
[H-].[Na+].OC[CH:5]1[O:9][CH:8]([C:10]2[CH:15]=[CH:14]C=CC=2)[N:7]([CH:16]([CH3:18])C)C1.ClC1C=C(C)C=CN=1>CN(C)C=O>[CH3:5][O:9][C:8]1[CH:10]=[C:15]([CH3:14])[CH:18]=[CH:16][N:7]=1

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 772482-Chloro-4-methylpyridineHCID 125661982-Phenyl-3-isopropyl-5-hydroxymethyloxazolidine

生成物 1

HCID 142234722-Methoxy-4-methylpyridine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
40 °C

実験手順

4.8 g of sodium hydride dispersion (55% strength) are cautiously added in portions to a solution of 27.5 g of 5-hydroxymethyl-3-isopropyl-2-phenyl-oxazolidine in 100 ml of dimethylformamide at 20°-40° C. and after foaming has ceased the mixture is stirred for a further 1-2 hours at 40° C. 12.7 g of 2-chloro-4-methyl-pyridine are then added and the reaction mixture is stirred for 2 hours at 80° C. After evaporating off the solvent in vacuo, the evaporation residue is taken up in ether and the ether solution is washed with water, dried over magnesium sulphate and evaporated in vacuo. Crude 2-[3'-isopropyl]-2'-phenyl-oxazolidinyl-(5')]-methoxy-4-methyl-pyridine is thus obtained.

後処理

  1. stirringthe reaction mixture is stirred for 2 hours at 80° C
  2. customAfter evaporating off the solvent in vacuo
  3. washthe ether solution is washed with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-05f2083f77754e04bea7357ae42a2194
出典データセット
uspto-grants-1983_10
特許番号
US04410530

反応ノート

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