Potassium Fluoride → HCID 178437211、化合物

HRID 45871

反応式

HRID 45871 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 178437211HCID 178437211、化合物収率 67%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-c07ad4186b054ea08a4e12d01fe6befb
出典データセット
uspto-grants-2013_09
特許番号
US08541575B2

関連ノート

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