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Bromine → 2-Bromo-1-(2,3-dichloro-4-(2-isopropyl-phenylsulfanyl)-phenyl)-ethanone

HRID 1005793
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HRID 1005793 반응식
[Br:1]Br.[Cl:3][C:4]1[C:9]([Cl:10])=[C:8]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[CH:18]([CH3:20])[CH3:19])[CH:7]=[CH:6][C:5]=1[C:21](=[O:23])[CH3:22]>O1CCOCC1>[Br:1][CH2:22][C:21]([C:5]1[CH:6]=[CH:7][C:8]([S:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[CH:18]([CH3:20])[CH3:19])=[C:9]([Cl:10])[C:4]=1[Cl:3])=[O:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24408BromineHCID 219067491-(2,3-Dichloro-4-(2-isopropyl-phenylsulfanyl)-phenyl)-ethanone

생성물 1

HCID 219067782-Bromo-1-(2,3-dichloro-4-(2-isopropyl-phenylsulfanyl)-phenyl)-ethanone

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

Then 2-bromo-1-(2,3-dichloro-4-(2-isopropyl-phenylsulfanyl)-phenyl)-ethanone 41 was prepared as follows. A solution of Br2 (50 mg) in dioxane (1.0 ml) was added to a solution of compound 40 (100 mg, 0.3 mmole) in 2 ml of dioxane. The solution was then stirred for another 10 minutes and concentrated. The residue was dissolved in EtOAc and purified on a 5-g silica gel cartridge, giving the desired product 41 as a white solid. 136 mg, ˜100%. 1H-NMR (CDCl3, 500 MHz) δ 1.19 (d, J=8.5 Hz, 6H), 3.43 (heptet, J=8.5 Hz, 1H), 4.45 (s, 2H), 6.42 (d, J=8.4 Hz, 1H), 7.19 (d, J=8.4 Hz, 1H), 7.25-7.31 (m, 1H), 7.49-7.54 (m, 3H); MS (DCI/NH3) m/z 436 (M+NH4)+.

후처리

  1. customThen 2-bromo-1-(2,3-dichloro-4-(2-isopropyl-phenylsulfanyl)-phenyl)-ethanone 41 was prepared
  2. concentrationconcentrated
  3. dissolutionThe residue was dissolved in EtOAc
  4. custompurified on a 5-g silica gel cartridge

출처 및 근거

ORD 기록
ord-afa6cf025d6143bb8c430101a88d07b8
출처 데이터셋
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06787542B2

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