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Water → HCID 15380615, 화합물

HRID 1421880
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HRID 1421880 반응식
[Cl:1]N1C(=O)CCC1=O.[Cl:9][C:10]1[C:15]([CH3:16])=[C:14]([Cl:17])[CH:13]=[CH:12][C:11]=1[S:18]([Cl:21])(=[O:20])=[O:19].O>ClC(Cl)C(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Cl:1][CH2:16][C:15]1[C:10]([Cl:9])=[C:11]([S:18]([Cl:21])(=[O:20])=[O:19])[CH:12]=[CH:13][C:14]=1[Cl:17]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 962WaterHCID 31398ChlorosuccinimideHCID 157253742,4-Dichloro-3-methylbenzene-1-sulfonyl chloride

생성물 1

HCID 15380615HCID 15380615, 화합물수율 11.6%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 65911,1,2,2-Tetrachloroethane
용매

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온도
120 °C

실험 절차

10 g (0.075 mol) of N-chlorosuccinimide and 30 mg of benzoyl peroxide are added to a solution of 6.5 g (0.025 mol) of 2,4-dichloro-3-methylbenzenesulfonyl chloride in 30 ml of 1,1,2,2-tetrachloroethane at room temperature and under a nitrogen atmosphere. The reaction mixture is heated at 120° C. for 3 hours, cooled to room temperature, poured into water and then extracted with dichloromethane. The organic phase is washed with water, with saturated sodium bicarbonate solution and finally with water until the washings are neutral. It is then dried over magnesium sulfate and concentrated under reduced pressure. Recrystallization from hexane gives 0.85 g of the expected product in the form of white crystals (yield=11.5%).

후처리

  1. temperaturecooled to room temperature
  2. extractionextracted with dichloromethane
  3. washThe organic phase is washed with water, with saturated sodium bicarbonate solution and finally with water until the washings
  4. dry with materialIt is then dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customRecrystallization from hexane

출처 및 근거

ORD 기록
ord-3b488a3544e643acb9ded9eaf310385a
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06080758

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