Triacetoxyperiodinane → HCID 59278091、化合物

HRID 1698223

反応式

HRID 1698223 の反応式
[C:1]1([CH3:19])[CH:6]=[CH:5][C:4]([S:7]([N:10]2[CH:14]=[CH:13][C:12]([CH:15]([OH:18])[CH2:16][CH3:17])=[N:11]2)(=[O:9])=[O:8])=[CH:3][CH:2]=1.CC(OI1(OC(C)=O)(OC(C)=O)OC(=O)C2C=CC=CC1=2)=O>C(Cl)Cl>[C:1]1([CH3:19])[CH:2]=[CH:3][C:4]([S:7]([N:10]2[CH:14]=[CH:13][C:12]([C:15](=[O:18])[CH2:16][CH3:17])=[N:11]2)(=[O:9])=[O:8])=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 159087TriacetoxyperiodinaneHCID 592783481-[1-(toluene-4-sulfonyl)-1H-pyrazol-3-yl]-propan-1-ol

生成物 1

HCID 59278091HCID 59278091、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1-[1-(toluene-4-sulfonyl)-1H-pyrazol-3-yl]-propan-1-ol (2.20 g, 7.85 mmol) in CH2Cl2 was added the Dess-Martin periodinane (4.24 g, 10.00 mmol). After 12 hours, the reaction was quenched with saturated aqueous sodium bicarbonate and filtered through diatomaceous earth and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 30% EtOAc in heptane. The major fractions were combined and the solvent was concentrated in vacuo to afford 1-[1-(toluene-4-sulfonyl)-1H-pyrazol-3-yl]-propan-1-one.

後処理

  1. customthe reaction was quenched with saturated aqueous sodium bicarbonate
  2. filtrationfiltered through diatomaceous earth
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by silica gel chromatography
  5. washeluting with 30% EtOAc in heptane
  6. concentrationthe solvent was concentrated in vacuo

出典と根拠

ORDレコード
ord-f531b9f9851e4737a995a3602735c253
出典データセット
uspto-grants-2012_04
特許番号
US08163918B2

関連ノート

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