N-bromobutanimide → HCID 59299491、化合物

HRID 1013802ノート

反応式

HRID 1013802 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 59299491HCID 59299491、化合物収率 97.2%

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-35f8228324a449c0ae534574be6b9923
出典データセット
uspto-grants-2011_07
特許番号
US07981918B2

反応ノート

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