Potassium Fluoride → HCID 178437211, 화합물

HRID 1843658

반응식

HRID 1843658 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 (CH2Cl2-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 (CH2Cl2-CH3COCH3 9/1)

출처 및 근거

ORD 기록
ord-9c6642fca7364a53afa1170ce7712230
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946250B2

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