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

HRID 1353111노트

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HRID 1353111 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6327Methyl Chloride용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-10643c8201fd4ce6a458cad26198adc2
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07220863B2

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