Water → HCID 15635484, 화합물

HRID 2116509노트

반응식

HRID 2116509 반응식
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

참가 물질

6

반응물 3

HCID 962WaterHCID 1087942-Iodoxybenzoic acidHCID 69220218HCID 69220218, 화합물

생성물 1

HCID 15635484HCID 15635484, 화합물수율 180.9%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5a47e1388ac34e69a32a7de7bfd55a4a
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07439232B2

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