HCID 22176567、化合物 → HCID 22176564、化合物

HRID 1797193ノート

反応式

HRID 1797193 の反応式
[OH:1][C:2]([C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-])=O)=[CH:14][CH:13]=1)([CH3:11])[CH2:3][NH:4][S:5]([CH:8]([CH3:10])[CH3:9])(=[O:7])=[O:6].[H][H]>C(OCC)(=O)C.[Pd]>[NH2:18][C:15]1[CH:14]=[CH:13][C:12]([C:2]([OH:1])([CH3:11])[CH2:3][NH:4][S:5]([CH:8]([CH3:9])[CH3:10])(=[O:7])=[O:6])=[CH:17][CH:16]=1

参加物

5

反応物 2

HCID 22176567HCID 22176567、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 22176564HCID 22176564、化合物収率 42%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

900 mg of [2-hydroxy-2-(4-nitrophenyl)propyl][(methylethyl)sulfonyl]amine and 1.2 equivalence of 10% Pd/C in ethyl acetate (50 mL) were subjected to a hydrogen atmosphere while shaking at 60 psi for 3 hours. Solution was filtered through a Celite® mat and the resulting filtrate was concentrated under reduced vacuum to yield 720 mg as an oil. This material was purified via silica gel chromatography employing the Chromatotron and using a 4000 micron rotor while eluting with a solvent of hexane/ethyl acetate 1:1 to yield the intermediate title compound (340 mg, 42%) as a tan solid. Ion spray M.S. 271.4 (M*−1).

後処理

  1. filtrationSolution was filtered through a Celite® mat
  2. concentrationthe resulting filtrate was concentrated under reduced vacuum
  3. customto yield 720 mg as an oil
  4. customThis material was purified via silica gel chromatography
  5. washwhile eluting with a solvent of hexane/ethyl acetate 1:1

出典と根拠

ORDレコード
ord-1f39119d00e942d5b93415f20f62844e
出典データセット
uspto-grants-2006_04
特許番号
US07034045B1

反応ノート

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