m-Chloroperbenzoic acid → UK-333747

HRID 842662노트

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HRID 842662 반응식
ClC1C=C(C=CC=1)C(OO)=[O:6].[Cl:12][C:13]1[C:14]([N:26]2[C:30]([C:31]3[CH:32]=[N:33][CH:34]=[CH:35][CH:36]=3)=[N:29][N:28]=[C:27]2[CH2:37][O:38][CH3:39])=[C:15]2[C:20](=[CH:21][C:22]=1[Cl:23])[NH:19][C:18](=[O:24])[C:17](=[O:25])[NH:16]2>CC(C)=O>[Cl:12][C:13]1[C:14]([N:26]2[C:30]([C:31]3[CH:32]=[N+:33]([O-:6])[CH:34]=[CH:35][CH:36]=3)=[N:29][N:28]=[C:27]2[CH2:37][O:38][CH3:39])=[C:15]2[C:20](=[CH:21][C:22]=1[Cl:23])[NH:19][C:18](=[O:24])[C:17](=[O:25])[NH:16]2

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 9802164HCID 9802164, 화합물

생성물 1

HCID 9867605UK-333747수율 17%

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

A solution of 3-chloroperoxybenzoic acid (0.85 g, 4.93 mmol) in acetone (20 ml) was added in one portion to a suspension of (−)-6,7-dichloro-5-[3-methoxymethyl-5-(3-pyridyl)-4H-1,2,4-triazol-4-yl]-2,3(1H,4H)-quinoxalinedione (see Example 111) (1.0 g, 2.24 mmol) in acetone (40 ml) which caused all the solid to dissolve. The reaction was stirred at room temperature for 40 minutes after which time a white solid began to form. The reaction mixture was allowed to stir at room temperature for 3 days. The white solid was collected by filtration and purified by flash chromatography on silica gel using dichloromethane:methanol:glacial acetic acid (90:10:1, by volume) as eluent, to give after combination and concentration of the appropriate fractions, the title compound (0.16 g, 17%) as a white solid, m.p. >310° C.

후처리

  1. dissolutionto dissolve
  2. customto form
  3. stirringto stir at room temperature for 3 days
  4. filtrationThe white solid was collected by filtration
  5. custompurified by flash chromatography on silica gel
  6. custommethanol:glacial acetic acid (90:10:1, by volume) as eluent, to give after combination and concentration of the appropriate fractions

출처 및 근거

ORD 기록
ord-892870667f4842d4ac1726a116b620c0
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06376490B1

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