N-bromobutanimide → HCID 59299491, 화합물

HRID 1013802노트

반응식

HRID 1013802 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([CH3:9])[C:3]=1[Cl:10].[Br:11]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[C:4]([CH2:9][Br:11])[C:3]=1[Cl:10]

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 148011751-Bromo-2,4-dichloro-3-methylbenzene

생성물 1

HCID 59299491HCID 59299491, 화합물수율 97.2%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 5943Carbon Tetrachloride용매

반응 조건

온도
0 °C

실험 절차

Treat a mixture of 1-bromo-2,4-dichloro-3-methyl-benzene (76.01 g, 0.316 mol) and N-bromosuccinimide (59.2 g, 0.332 mol) in CCl4 (500 mL) with benzoyl peroxide (0.77 g, 3.18 mmol) and is heat to reflux for 6 hours under N2. Cool the reaction mixture to 0° C. and filter using hexanes to rinse the solids. Extract the filtrate with water and saturated NaHCO3. Dry the organic layer (Na2SO4) and remove the solvent in vacuo to afford 97.89 g (97%) of the titled product. Rf=0.34 (100% hexanes).

후처리

  1. additionTreat
  2. temperatureis heat
  3. temperatureto reflux for 6 hours under N2
  4. filtrationfilter
  5. washto rinse the solids
  6. extractionExtract the filtrate with water and saturated NaHCO3
  7. dry with materialDry the organic layer (Na2SO4)
  8. customremove the solvent in vacuo

출처 및 근거

ORD 기록
ord-35f8228324a449c0ae534574be6b9923
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07981918B2

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