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Hydrogen Peroxide → HCID 86584037, 화합물

HRID 2306072
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HRID 2306072 반응식
OO.FC(F)(F)C(OC(=O)C(F)(F)F)=[O:6].[F:16][C:17]1[CH:18]=[C:19]([N:33]2[CH2:37][C@H:36]([CH2:38][NH:39][C:40](=[O:42])[CH3:41])[O:35][C:34]2=[O:43])[CH:20]=[CH:21][C:22]=1[N:23]1[CH2:28][CH2:27][N:26]([S:29]([CH3:32])(=[O:31])=[O:30])[CH2:25][CH2:24]1>C(Cl)Cl>[F:16][C:17]1[CH:18]=[C:19]([N:33]2[CH2:37][C@@H:36]([CH2:38][NH+:39]([O-:6])[C:40](=[O:42])[CH3:41])[O:35][C:34]2=[O:43])[CH:20]=[CH:21][C:22]=1[N:23]1[CH2:28][CH2:27][N:26]([S:29]([CH3:32])(=[O:31])=[O:30])[CH2:25][CH2:24]1
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참가 물질

5

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HCID 784Hydrogen PeroxideHCID 9845Trifluoroacetic anhydrideHCID 10431934N-[[(5S)-3-[3-Fluoro-4-[4-(methylsulfonyl)-1-piperazinyl]phenyl]-2-oxo-5-oxazolidinyl]methyl]acetamide

생성물 1

HCID 86584037HCID 86584037, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

Pertrifluoroacetic acid is prepared in situ by the addition of 30% H2O2 solution (0.15 mL) to trifluoroacetic anhydride (0.45 mL) in 5 mL of methylene chloride at 0° C. This solution is stirred at 0° C. for ten minutes, at 25° C. for 30 minutes and then cooled back to 0° C. (S)-N-[[3-[3-fluoro-4-[4-(methylsulfonyl)-1-piperazinyl]phenyl]-2-oxo-5-oxazolidinyl]-methyl]acetamide (VIII-G, R1=COCH3, R9=CH3, X1=F, X2=H) (0.207 g) is added and the reaction is stirred at 25° C. for 30 minutes and then concentrated. The residue is chromatographed on silica gel using 10% methanol (saturated with ammonia) in chloroform as the eluent to afford 0.14 g of the N-oxide as a hydrate.

후처리

  1. additionis added
  2. stirringthe reaction is stirred at 25° C. for 30 minutes
  3. concentrationconcentrated
  4. customThe residue is chromatographed on silica gel using 10% methanol (saturated with ammonia) in chloroform as the eluent

출처 및 근거

ORD 기록
ord-22ea2b5e029a4c63bf513ae67083f1af
출처 데이터셋
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06441188B1

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