Picolyl chloride hydrochloride → 2-(Methoxymethyl)pyridine

HRID 1076366노트

반응식

HRID 1076366 반응식
Cl.Cl[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][N:5]=1.[CH3:10][O-:11].[Na+]>CO>[CH3:10][O:11][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][N:5]=1

참가 물질

4

반응물 2

HCID 23392Picolyl chloride hydrochlorideHCID 10942334Sodium Methoxide

생성물 1

HCID 2532202-(Methoxymethyl)pyridine

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-(Chloromethyl)pyridine hydrochloride (16.3 g., 0.1 mole) is dissolved in 100 ml. of methanol. Freshly prepared sodium methoxide (5 g., 0.22 mole of sodium dissolved in 150 ml. of methanol) is added dropwise. The resulting mixture is heated at reflux for 18 hours, then filtered. The filtrate is concentrated. Water and ether are added, the aqueous phase is extracted with ether and the combined ethereal phases are washed with water and saturated aqueous sodium chloride, then dried over magnesium sulfate, concentrated and distilled to give 2-(methoxymethyl)pyridine.

후처리

  1. temperatureThe resulting mixture is heated
  2. temperatureat reflux for 18 hours
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated
  5. additionWater and ether are added
  6. extractionthe aqueous phase is extracted with ether
  7. washthe combined ethereal phases are washed with water and saturated aqueous sodium chloride
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated
  10. distillationdistilled

출처 및 근거

ORD 기록
ord-1d48ab535ad4491d97f358a9c06b451c
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03956494

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