Sodium hydride → 2-Methoxy-4-methylpyridine

HRID 647984노트

반응식

HRID 647984 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 142234722-Methoxy-4-methylpyridine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-05f2083f77754e04bea7357ae42a2194
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410530

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