(6-(2-Methoxyethoxy)pyridin-3-yl)methanol → 6-(2-Methoxyethoxy)nicotinaldehyde

HRID 603216노트

반응식

HRID 603216 반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[N:11]=[CH:10][C:9]([CH2:12][OH:13])=[CH:8][CH:7]=1>C1(C)C=CC=CC=1.O=[Mn]=O>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[CH:8][C:9]([CH:12]=[O:13])=[CH:10][N:11]=1

참가 물질

4

반응물 1

HCID 15067095(6-(2-Methoxyethoxy)pyridin-3-yl)methanol

생성물 1

HCID 150670976-(2-Methoxyethoxy)nicotinaldehyde수율 82.8%

시약·촉매·용매 2

HCID 14801Manganese dioxide촉매HCID 1140Toluene용매

실험 절차

[6-(2-methoxyethoxy)pyridine-3-yl]methanol (1.83 g 10.0 mmol) was dissolved in toluene (50 ml) and heated to reflux under an air condenser. Finely powdered MnO2 (4.0 g) was added portion wise over 2 hours. After a further 2 and a half hours of heating the mixture was taken off the boil allowed to cool slightly then filtered through celite and washed with toluene. The filtrate was concentrated in-vacuo to yield a pale yellow oil which crystallized under high vacuum to yield the crude product (1.50 g).

후처리

  1. temperatureheated
  2. temperatureto reflux under an air condenser
  3. temperatureAfter a further 2 and a half hours of heating the mixture
  4. temperatureto cool slightly
  5. filtrationthen filtered through celite
  6. washwashed with toluene
  7. concentrationThe filtrate was concentrated in-vacuo
  8. customto yield a pale yellow oil which
  9. customcrystallized under high vacuum

출처 및 근거

ORD 기록
ord-904aa952aa314134a24c090c773a39b6
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906645B2

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