Dimethylamine → 2-Dimethylaminomethyl-3-hydroxy-4-methylpyridine

HRID 904142노트

반응식

HRID 904142 반응식
[OH:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH3:8].[CH3:9][NH:10][CH3:11].[CH2:12]=O>O>[CH3:9][N:10]([CH2:12][C:3]1[C:2]([OH:1])=[C:7]([CH3:8])[CH:6]=[CH:5][N:4]=1)[CH3:11]

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 712FormaldehydeHCID 27629084-Methylpyridin-3-ol

생성물 1

HCID 233337992-Dimethylaminomethyl-3-hydroxy-4-methylpyridine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution consisting of 3-hydroxy-4-methylpyridine (32.7 g.), 30% aqueous dimethylamine (46.5 ml.) and formalin (25 ml.) in water (50 ml.) was heated on a steam bath for a period of two hours. The cooled reaction solution was then extracted with ten-100 ml. portions of diethyl ether and the combined ether and extracts were subsequently dried over anhydrous magnesium sulfate and filtered. After removal of the volatile liquids by means of evaporation under reduced pressure, there was finally obtained an oil as residue which was subsequently distilled in vacuo to give pure 2-dimethylaminomethyl-3-hydroxy-4-methylpyridine (yield, 34.5 g.), b.p. 71°-74° C./0.6 mm. Hg. The corresponding dihydrochloride salt melted at 214°-217° C. (decomp.) after recrystallization from ethanol/diethyl ether.

후처리

  1. temperaturewas heated on a steam bath for a period of two hours
  2. customThe cooled reaction solution
  3. extractionwas then extracted with ten-100 ml
  4. dry with materialportions of diethyl ether and the combined ether and extracts were subsequently dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customAfter removal of the volatile liquids
  7. customby means of evaporation under reduced pressure, there
  8. customwas finally obtained an oil as residue which
  9. distillationwas subsequently distilled in vacuo

출처 및 근거

ORD 기록
ord-8dd41e8122944b6d8ab142ac3bc4b7ca
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04230714

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