Potassium Fluoride → 5-Chloro-3-ethynylpyridin-2-amine

HRID 490448

반응식

HRID 490448 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]#[C:10][Si](C)(C)C)[C:5]([NH2:8])=[N:6][CH:7]=1.[F-].[K+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]#[CH:10])[C:5]([NH2:8])=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 522689Potassium FluorideHCID 247294655-Chloro-3-((trimethylsilyl)ethynyl)pyridin-2-amine

생성물 1

HCID 259186675-Chloro-3-ethynylpyridin-2-amine수율 89.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A suspension of 1.6 g of 5-chloro-3-trimethylsilanylethynylpyridin-2-ylamine and 1.24 g of potassium fluoride in 80 ml of methanol is brought to reflux for approximately 3 hours 30 minutes. After returning to a temperature in the region of 20° C., the mixture is filtered through celite, and the insoluble material is washed three times with 50 ml of methanol. The filtrate is concentrated to dryness under reduced pressure (13 kPa). The residue is taken up with 100 ml of dichloromethane. The solution obtained is washed with three times 60 ml of water, dried over magnesium sulfate, filtered, and concentrated to dryness under reduced pressure (13 kPa). 0.97 g of 5-chloro-3-ethynylpyridin-2-ylamine is thus obtained in the form of a solid, the characteristics of which are as follows:

후처리

  1. temperatureto reflux for approximately 3 hours 30 minutes
  2. customAfter returning to a temperature in the region of 20° C.
  3. filtrationthe mixture is filtered through celite
  4. washthe insoluble material is washed three times with 50 ml of methanol
  5. concentrationThe filtrate is concentrated to dryness under reduced pressure (13 kPa)
  6. customThe solution obtained
  7. washis washed with three times 60 ml of water
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated to dryness under reduced pressure (13 kPa)

출처 및 근거

ORD 기록
ord-fbb17af726ac46589fe669405f1ad55a
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07528147B2

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