Acetic Acid → 4-Chloro-3,5-difluoro-2-(1-hydroxy-2-propyl)pyridine

HRID 1080214노트

반응식

HRID 1080214 반응식
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][N:5]=[C:4]([CH:9]([CH3:18])[CH2:10][O:11]C2CCCCO2)[C:3]=1[F:19].O.C(O)(=O)C>C1COCC1>[Cl:1][C:2]1[C:7]([F:8])=[CH:6][N:5]=[C:4]([CH:9]([CH3:18])[CH2:10][OH:11])[C:3]=1[F:19]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 962WaterHCID 540115134-Chloro-3,5-difluoro-2-(1-(2-tetrahydropyranyl)oxy-2-propyl)pyridine

생성물 1

HCID 543283394-Chloro-3,5-difluoro-2-(1-hydroxy-2-propyl)pyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
45 °C

실험 절차

The product of Step 1 is dissolved in 200 mL of 2:1 THF:water and to this solution is added 6 mL of acetic acid. The reaction mixture is heated at 45° C. for approximately 5 hours. The THF is removed under reduced pressure and the aqueous reaction mixture is adjusted to a pH in the range of 8 to 9 with 10% sodium carbonate and is then extracted with methylene chloride. The organic layer is dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford the title compound.

후처리

  1. customThe THF is removed under reduced pressure
  2. extractionis then extracted with methylene chloride
  3. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-22d870fc6965446d8037cd85e3adeaac
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05580872

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