Potassium Fluoride → HCID 178437211, 화합물

HRID 45871

반응식

HRID 45871 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([C:10]2[C:14]([C:15]#[C:16][Si](C)(C)C)=[CH:13][NH:12][N:11]=2)[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[F-].[K+]>CO>[C:15]([C:14]1[C:10]([C:6]2[CH:7]=[CH:8][CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)=[N:11][NH:12][CH:13]=1)#[CH:16]

참가 물질

4

반응물 2

HCID 522689Potassium FluorideHCID 1785041883-(3-nitrophenyl)-4-[(trimethylsilyl)ethynyl]-1H-pyrazole

생성물 1

HCID 178437211HCID 178437211, 화합물수율 67%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

300 mg (1.05 mmol) of 3-(3-nitrophenyl)-4-[(trimethylsilyl)ethynyl]-1H-pyrazole were suspended in 60 ml of methanol and 120 mg (2.1 mmol) of potassium fluoride were added and the mixture stirred at room temperature overnight. After this time the solvent was removed under reduced pressure and the residue taken up with dichloromethane and washed with water. The organic layer was then dried over sodium sulphate and evaporated. The crude was finally purified by flash-chromatography on a silica gel column (CH2C12-CH3COCH3 9/1), giving 150 mg (67%) of the title compound.

후처리

  1. customAfter this time the solvent was removed under reduced pressure
  2. washwashed with water
  3. dry with materialThe organic layer was then dried over sodium sulphate
  4. customevaporated
  5. customThe crude was finally purified by flash-chromatography on a silica gel column (CH2C12-CH3COCH3 9/1)

출처 및 근거

ORD 기록
ord-c07ad4186b054ea08a4e12d01fe6befb
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541575B2

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