Carbon Tetrachloride → HCID 12274172, 화합물

HRID 355423노트

반응식

HRID 355423 반응식
[Br:1]N1C(=O)CCC1=O.[CH3:9][C:10]1[CH:23]=[CH:22][C:21]2[O:20][C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[C:13](=[O:24])[C:12]=2[CH:11]=1.C(Cl)(Cl)(Cl)Cl>C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.O>[Br:1][CH2:9][C:10]1[CH:23]=[CH:22][C:21]2[O:20][C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[C:13](=[O:24])[C:12]=2[CH:11]=1

참가 물질

6

반응물 3

HCID 5943Carbon TetrachlorideHCID 67184N-bromobutanimideHCID 2234732-Methylxanthen-9-one

생성물 1

HCID 12274172HCID 12274172, 화합물수율 71.3%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 962Water용매

실험 절차

Benzoyl peroxide (4.6 g, 19 mmol) and N-bromosuccinimide (67.6 g, 380 mmol) were added to a mixture of 2-methyl-9H-xanthen-9-one (79.9 g, 380 mmol) and carbon tetrachloride (800 ml) with heating under reflux, and the mixture was stirred for 4 hours. After spontaneous cooling to room temperature, water was added to the reaction mixture, and the reaction product was extracted with chloroform. The extract was washed with saturated sodium bicarbonate aqueous solution, water and saturated sodium chloride aqueous solution in that order, dried over anhydrous magnesium sulfate, and then concentrated under a reduced pressure. The resulting residue was recrystallized from ethyl acetate to give the title compound (78.3 g, 271 mmol, 71%) as yellow crystals.

후처리

  1. temperaturewith heating
  2. temperatureunder reflux
  3. extractionthe reaction product was extracted with chloroform
  4. washThe extract was washed with saturated sodium bicarbonate aqueous solution, water and saturated sodium chloride aqueous solution in that order
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under a reduced pressure
  7. customThe resulting residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-3c3626e484a442759f6aeddab0aca5e9
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05830902

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