Dimethylamine → 2-Dimethylamino-4-hydroxymethyl-3,5,6-trifluoropyridine

HRID 256163노트

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HRID 256163 반응식
[OH:1][CH2:2][C:3]1[C:8]([F:9])=[C:7](F)[N:6]=[C:5]([F:11])[C:4]=1[F:12].[CH3:13][NH:14][CH3:15].O>C(O)C>[CH3:13][N:14]([CH3:15])[C:7]1[C:8]([F:9])=[C:3]([CH2:2][OH:1])[C:4]([F:12])=[C:5]([F:11])[N:6]=1

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 962WaterHCID 139851584-Hydroxymethyl-2,3,5,6-tetrafluoropyridine

생성물 1

HCID 139851642-Dimethylamino-4-hydroxymethyl-3,5,6-trifluoropyridine수율 87.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1.0 g (0.0055 mole) of 4-hydroxymethyl-2,3,5,6-tetrafluoropyridine (from Example 5) and 0.23 g (0.0050 mole) of dimethylamine in 25 ml of ethanol was refluxed for approximately twenty hours. The reaction mixture was cooled and was poured into water. This mixture was extracted with diethyl ether. The extract was dried over anhydrous magnesium sulfate, filtered, and the solvent evaporated under reduced pressure, yielding 0.9 g of 2-dimethylamino-4-hydroxymethyl-3,5,6-trifluoropyridine as a yellow oil. The structure and nmr spectra are set forth in Table 1C below.

후처리

  1. temperaturewas refluxed for approximately twenty hours
  2. temperatureThe reaction mixture was cooled
  3. extractionThis mixture was extracted with diethyl ether
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customthe solvent evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-441e0d58445b4beaa592252f1f6fb227
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04701464

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