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Water → HCID 53244623, 화합물

HRID 511915
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HRID 511915 반응식
[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=1[C:9](Cl)=[O:10])=[O:5])[CH3:2].[C:16]1([C:22]([O:24][OH:25])=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.N1C=CC=CC=1.O>C(Cl)(Cl)Cl.ClCCl>[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=1[C:9]([O:25][O:24][C:22](=[O:23])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:10])=[O:5])[CH3:2]
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참가 물질

7

반응물 4

HCID 962WaterHCID 1049PyridineHCID 523077Perbenzoic acidHCID 86675009HCID 86675009, 화합물

생성물 1

HCID 53244623HCID 53244623, 화합물수율 75.7%

시약·촉매·용매 2

HCID 6212Chloroform용매
HCID 6344
Dichloromethane
용매

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온도
-18 °C

실험 절차

8.6 g (67 mmol) of 2-(ethoxycarbonyloxy)benzoyl chloride (obtained in Example 1.2) and 10.2 g (44 mmol) of benzenecarboperoxoic acid are dissolved in 43 ml of chloroform. The mixture is cooled to −18° C. and then 2.2 ml (38 mmol) of pyridine in 5 ml of dichloromethane are added dropwise. After stirring at −18° C. for 2 hours, water is added and the mixture is extracted with dichloromethane. The organic phase is dried over magnesium sulphate, filtered and then concentrated. The residue is purified by chromatography on silica gel eluted with a pentane/dichloromethane 5/5 mixture. 11 g of (2-(ethoxycarbonyloxy)benzoyl)benzoyl peroxide are obtained in the form of a beige solid with a yield of 75%.

후처리

  1. extractionthe mixture is extracted with dichloromethane
  2. dry with materialThe organic phase is dried over magnesium sulphate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue is purified by chromatography on silica gel
  6. washeluted with a pentane/dichloromethane 5/5 mixture

출처 및 근거

ORD 기록
ord-2df086326bd64c78acdd05ad96490f62
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09102607B2

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