1-Propanol → (3,5,6-Trifluoro-2-pyridyl)hydrazine

HRID 1353111ノート

反応式

HRID 1353111 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4](F)[N:3]=1.O.[NH2:12][NH2:13].C(O)CC>ClC>[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([NH:12][NH2:13])[N:3]=1

参加物

5

反応物 3

HCID 10311-PropanolHCID 24654Hydrazine hydrate (1:1)HCID 1377492,3,5,6-Tetrafluoropyridine

生成物 1

HCID 21551824(3,5,6-Trifluoro-2-pyridyl)hydrazine収率 83.8%

試薬・触媒・溶媒 1

HCID 6327Methyl Chloride溶媒

反応条件

温度
80 °C

実験手順

23.2 g of the compound obtained in Step 1 and 37.3 ml of hydrazine monohydrate were added to 100 ml of n-propanol, and the resulting mixture was heated to 80° C. for 2 hours. The reaction mixture was distilled under a reduced pressure to remove the solvent. The residue thus obtained was dissolved in 100 ml of chloromethane, washed with water, and dried over anhydrous magnesium sulfate. The dried organic layer was concentrated under a reduced pressure to obtain 21.9 g (yield: 83.8%) of the title compound as a light yellow solid.

後処理

  1. distillationThe reaction mixture was distilled under a reduced pressure
  2. customto remove the solvent
  3. customThe residue thus obtained
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationThe dried organic layer was concentrated under a reduced pressure

出典と根拠

ORDレコード
ord-10643c8201fd4ce6a458cad26198adc2
出典データセット
uspto-grants-2007_05
特許番号
US07220863B2

反応ノート

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