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

HRID 256163ノート

反応式

HRID 256163 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-441e0d58445b4beaa592252f1f6fb227
出典データセット
uspto-grants-1987_10
特許番号
US04701464

反応ノート

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