Water → HCID 15635484、化合物

HRID 2116509ノート

反応式

HRID 2116509 の反応式
I(C1C=CC=CC=1C(O)=O)(=O)=O.C(C1C=CC(C([C:23]2[CH:28]=[CH:27][N:26]=[CH:25][C:24]=2[O:29][CH2:30][O:31][CH2:32][CH2:33][Si:34]([CH3:37])([CH3:36])[CH3:35])O)=CC=1)C.O>CS(C)=O.O1CCCC1>[CH3:35][Si:34]([CH3:37])([CH3:36])[CH2:33][CH2:32][O:31][CH2:30][O:29][C:24]1[CH:25]=[N:26][CH:27]=[CH:28][CH:23]=1

参加物

6

反応物 3

HCID 962WaterHCID 1087942-Iodoxybenzoic acidHCID 69220218HCID 69220218、化合物

生成物 1

HCID 15635484HCID 15635484、化合物収率 180.9%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of o-iodoxybenzoic acid (IBX) in dimethyl sulfoxide (15 mL), a solution of (4-ethylphenyl)-[3-[2-(trimethylsilyl)ethoxymethoxy]pyridin-4-yl]-methanol (synthesized in Reference Example 6; 3.0 g, 8.34 mmol) in tetrahydrofuran (20 mL) was added and the reaction mixture was stirred at room temperature for 17.5 hours. Water was added to the reaction mixture and the resulting precipitate was filtered and washed with ethyl acetate. The filtrate was washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to give 4-(4-ethylbenzoyl)-[3-[2-(trimethylsilyl)ethoxymethoxy]pyridine (3.4 g).

後処理

  1. filtrationthe resulting precipitate was filtered
  2. washwashed with ethyl acetate
  3. washThe filtrate was washed with water and saturated aqueous sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-5a47e1388ac34e69a32a7de7bfd55a4a
出典データセット
uspto-grants-2008_10
特許番号
US07439232B2

反応ノート

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