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m-Chloroperbenzoic acid → 2-(6-Propylsulfinyl-2-pyridyl)-4H-1,3-benzothiazine-4-one

HRID 499306
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HRID 499306 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH2:12]([S:15][C:16]1[N:21]=[C:20]([C:22]2[S:23][C:24]3[CH:32]=[CH:31][CH:30]=[CH:29][C:25]=3[C:26](=[O:28])[N:27]=2)[CH:19]=[CH:18][CH:17]=1)[CH2:13][CH3:14]>C(OCC)(=O)C>[CH2:12]([S:15]([C:16]1[N:21]=[C:20]([C:22]2[S:23][C:24]3[CH:32]=[CH:31][CH:30]=[CH:29][C:25]=3[C:26](=[O:28])[N:27]=2)[CH:19]=[CH:18][CH:17]=1)=[O:9])[CH2:13][CH3:14]
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 22939404HCID 22939404, 화합물

생성물 1

HCID 229395302-(6-Propylsulfinyl-2-pyridyl)-4H-1,3-benzothiazine-4-one수율 76%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 3-chloroperbenzoic acid (ca. 50%, 0.17 g, 0.49 mmol) in ethyl acetate (20 ml) was added dropwise to a solution of 2-(6-propylthio-2-pyridyl)-4H-1,3-benzothiazine-4-one (0.15 g, 0.48 mmol), which was obtained in Example 59, in ethyl acetate (50 ml) with stirring. The reaction mixture was stirred at room temperature for 18 hrs, washed with saturated aqueous sodium hydrogen carbonate solution (50 ml×2) and saturated brine, dried (MgSO4) and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate to give the titled compound (0.12 g, 76%) as crystals.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 18 hrs
  2. washwashed with saturated aqueous sodium hydrogen carbonate solution (50 ml×2) and saturated brine
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-c45fab8a832d450889d6aa0a514deba2
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07767665B2

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