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m-Chloroperbenzoic acid → HCID 9817284, 화합물

HRID 1075467
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HRID 1075467 반응식
[CH2:1]([S:8][CH2:9][CH:10]([CH2:14][CH2:15][C:16]([OH:18])=[O:17])[C:11]([OH:13])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC1C=CC=C(C(OO)=[O:27])C=1>ClCCl>[CH2:1]([S:8]([CH2:9][CH:10]([CH2:14][CH2:15][C:16]([OH:18])=[O:17])[C:11]([OH:13])=[O:12])=[O:27])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acid2회HCID 15410800HCID 15410800, 화합물

생성물 1

HCID 9817284HCID 9817284, 화합물수율 69%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a cooled mixture (-78° C.) of 2-[(benzylsulfanyl)methyl]pentanedioic acid (5.2 g, 19.4 mmol) in dichloromethane (100 ml) was added 3-chloroperbenzoic acid (85%, 3.9 g, 19.4 mmol) with stirring. The reaction mixture was allowed to stir for 1 hour at -78° C., then allowed to warm to room temperature. If starting material was still present according to analysis by TLC, the reaction was cooled again to -78° C. and additional 3-chloroperbenzoic acid (2-4 mmol depending on the intensity of the starting material spot) added and the reaction mixture allowed to warm at room temperature. This was repeated until no more starting material was detected by TLC. The dichloromethane was removed under reduced pressure and the resulting residue was purified by column chromatography to yield 3.8 g (69%) of white solid.

후처리

  1. stirringto stir for 1 hour at -78° C.
  2. temperaturethe reaction was cooled again to -78° C.
  3. additionadded
  4. temperatureto warm at room temperature
  5. customThe dichloromethane was removed under reduced pressure
  6. customthe resulting residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-bc69059ad5634987aa4425981ef12ce9
출처 데이터셋
uspto-grants-1999_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05902817

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