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Phenyltrimethylammonium bromide dibromide → 2-Bromo-1-(3,5-dichloropyridin-2-yl)ethanone

HRID 55976
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HRID 55976 반응식
[Cl:1][C:2]1[C:3]([C:9](=[O:11])[CH3:10])=[N:4][CH:5]=[C:6]([Cl:8])[CH:7]=1.[Br-:12].[Br-].[Br-].C[N+](C)(C)C1C=CC=CC=1.C[N+](C1C=CC=CC=1)(C)C.C[N+](C1C=CC=CC=1)(C)C>O1CCCC1>[Br:12][CH2:10][C:9]([C:3]1[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][N:4]=1)=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 17977687Phenyltrimethylammonium bromide dibromideHCID 217121631-(3,5-Dichloropyridin-2-yl)ethanone

생성물 1

HCID 534166072-Bromo-1-(3,5-dichloropyridin-2-yl)ethanone수율 161.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 5.00 g of 1-(3,5-dichloropyridin-2-yl)ethanone in 75 ml of tetrahydrofuran, 9.94 g of trimethylphenylammonium tribromide was added, and the mixture was stirred at room temperature for 16 hours. After completion of the reaction, the precipitated solid was filtered off through celite, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 5:95 to 15:85) as the eluent to obtain 6.64 g of the desired product as a brown oil.

후처리

  1. customAfter completion of the reaction
  2. filtrationthe precipitated solid was filtered off through celite
  3. customthe solvent was evaporated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-cd850f646e874edab909d8c8af2c313c
출처 데이터셋
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09434684B2

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