Tetrabutylammonium Fluoride → 1-benzyl-1H-pyrazol-4-ol

HRID 1167363ノート

反応式

HRID 1167363 の反応式
[CH2:1]([N:8]1[CH:12]=[C:11]([O:13][Si](C(C)(C)C)(C)C)[CH:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC>C1COCC1>[CH2:1]([N:8]1[CH:12]=[C:11]([OH:13])[CH:10]=[N:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 2724141Tetrabutylammonium FluorideHCID 22996265HCID 22996265、化合物

生成物 1

HCID 6422181-benzyl-1H-pyrazol-4-ol収率 35%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

1-Benzyl-4-t-butyldimethylsilyloxypyrazole (3.0 g, 10.4 mmol) was dissolved in THF (20 ml) and tetrabutylammonium fluoride (52 ml of LM solution in THE) was added. The reaction was stirred overnight and the solvent removed in vacuo. The residue was dissolved in water and extracted into diethylether. The organics dried over sodium sulfate, and the ether removed in vacuo. The residue purified by column chromatography (silica gel, chloroform→2% methanol/chloroform) to yield product (0.63 g, 35%). MS

後処理

  1. customthe solvent removed in vacuo
  2. dissolutionThe residue was dissolved in water
  3. extractionextracted into diethylether
  4. dry with materialThe organics dried over sodium sulfate
  5. customthe ether removed in vacuo
  6. customThe residue purified by column chromatography (silica gel, chloroform→2% methanol/chloroform)

出典と根拠

ORDレコード
ord-33071fc89700440885a3dd14c2a9a74f
出典データセット
uspto-grants-2003_09
特許番号
US06617347B1

反応ノート

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