m-Chloroperbenzoic acid → HCID 59750307, 화합물

HRID 499292노트

반응식

HRID 499292 반응식
[CH3:1][S:2][C:3]1[N:8]=[C:7]([C:9]2[S:10][C:11]3[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=3[C:13](=[O:15])[N:14]=2)[CH:6]=[CH:5][CH:4]=1.ClC1C=CC=C(C(OO)=[O:28])C=1>C(Cl)(Cl)Cl>[CH3:1][S:2]([C:3]1[N:8]=[C:7]([C:9]2[S:10][C:11]3[CH:19]=[CH:18][CH:17]=[CH:16][C:12]=3[C:13](=[O:15])[N:14]=2)[CH:6]=[CH:5][CH:4]=1)=[O:28]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 22939568HCID 22939568, 화합물

생성물 1

HCID 59750307HCID 59750307, 화합물수율 64%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

2-(6-Methylthio-2-pyridyl)-4H-1,3-benzothiazine-4-one (0.28 g, 1.0 mmol) obtained in Example 43 was dissolved in chloroform (30 ml). To the stirred mixture was added dropwise a solution of 3-chloroperbenzoic acid (ca. 70%, 0.25 g, 1.0 mmol) in chloroform (10 ml). The reaction mixture was stirred for 1 hr and concentrated under reduced pressure. The residue was subjected to a silica gel column chromatography and eluted with 10% methanol-chloroform and recrystallized from ethanol to give the titled compound (0.19 g, 64%) as crystals.

후처리

  1. concentrationconcentrated under reduced pressure
  2. washeluted with 10% methanol-chloroform
  3. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-e7513221bce34e52b5121762f3d3ca71
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07767665B2

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