p-Bromoacetophenone → 4-Bromo-1-(1,3-dithian-2-yl)ethylbenzene

HRID 55628

반응식

HRID 55628 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH3:9])=[CH:4][CH:3]=1.[CH2:11]([SH:15])[CH2:12][CH2:13][SH:14].B(F)(F)F.[CH3:20]COCC>ClC(Cl)Cl.ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH:9]2[S:15][CH2:11][CH2:12][CH2:13][S:14]2)[CH3:20])=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 7466p-BromoacetophenoneHCID 8000Boron trifluoride etherateHCID 80131,3-Propanedithiol

생성물 1

HCID 219601124-Bromo-1-(1,3-dithian-2-yl)ethylbenzene

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6344Dichloromethane용매

실험 절차

To the compound p-bromoacetophenone (36.85 g, 185 mmol) in trichloromethane (300 ml) was added 1,3-propanedithiol (25 g, 230 mmol) and boron trifluoride etherate (3 ml). The resulting mixture was stirred at room temperature for 48 hours. The mixture was diluted with dichloromethane (500 ml), washed twice with 10% sodium hydroxide (200 ml), water, and brine, and then dried (Na2SO4). The product was concentrated to an oil. A portion was stirred with ether (100 ml) and a crystalline product was formed. The crystalline product was recovered by filtration and purified by recrystallization to yield 4-bromo-1-(1,3-dithian-2-yl)ethylbenzene.

후처리

  1. washwashed twice with 10% sodium hydroxide (200 ml), water, and brine
  2. dry with materialdried (Na2SO4)
  3. concentrationThe product was concentrated to an oil
  4. stirringA portion was stirred with ether (100 ml)
  5. customa crystalline product was formed
  6. filtrationThe crystalline product was recovered by filtration
  7. custompurified by recrystallization

출처 및 근거

ORD 기록
ord-6cb87811cba8461b8d090235ec7639ac
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624927

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