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m-Chloroperbenzoic acid → HCID 59750161, 화합물

HRID 499307
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HRID 499307 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[CH2:12]([S:15]([C:17]1[N:22]=[C:21]([C:23]2[S:24][C:25]3[CH:33]=[CH:32][CH:31]=[CH:30][C:26]=3[C:27](=[O:29])[N:28]=2)[CH:20]=[CH:19][CH:18]=1)=[O:16])[CH2:13][CH3:14]>C(OCC)(=O)C>[CH2:12]([S:15]([C:17]1[N:22]=[C:21]([C:23]2[S:24][C:25]3[CH:33]=[CH:32][CH:31]=[CH:30][C:26]=3[C:27](=[O:29])[N:28]=2)[CH:20]=[CH:19][CH:18]=1)(=[O:9])=[O:16])[CH2:13][CH3:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 229395302-(6-Propylsulfinyl-2-pyridyl)-4H-1,3-benzothiazine-4-one

생성물 1

HCID 59750161HCID 59750161, 화합물수율 41%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A solution of 3-chloroperbenzoic acid (ca. 50%, 0.44 g, 1.2 mmol) in ethyl acetate (10 ml) was added dropwise to a solution of 2-(6-propylsulfinyl-2-pyridyl)-4H-1,3-benzothiazine-4-one (0.20 g, 0.64 mmol), which was obtained in Example 60, 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 ethanol to give the titled compound (0.09 g, 41%) 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 ethanol

출처 및 근거

ORD 기록
ord-6bbda1dc407d4de3920414178f5d748d
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07767665B2

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