Benzoyl Peroxide → HCID 19046452、化合物

HRID 1757237ノート

反応式

HRID 1757237 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([CH3:12])[CH:8]=[C:9]([Cl:11])[CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[Br:13]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[C:1]([C:5]1[CH:6]=[C:7]([CH:8]=[C:9]([Cl:11])[CH:10]=1)[CH2:12][Br:13])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 190464341-tert-Butyl-3-chloro-5-methylbenzene

生成物 1

HCID 19046452HCID 19046452、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

3-t-Butyl-5-chlorotoluene (5.7 g) was dissolved in carbon tetrachloride (80 ml) and N-bromosuccinimide (5.56 g) was added followed by benzoyl peroxide (750 mg). This mixture was heated at reflux for 6h. The mixture was cooled, filtered through celite and the filtrate was concentrated in vacuo. The residue was purified by chromatography on silica using hexane as eluant. This afforded the title compound as a colourless liquid. 1H NMR (360 MHz, CDCl3) δ1.31 (9H, s, (CH3)3), 4.42 (2H, s, CH2), 7.20 (1H, t, J=1.5 Hz, ArH), 7.26 (1H, t, J=1.5 Hz, ArH), 7.28 (1H, t, J=1.5 Hz, ArH).

後処理

  1. temperatureThis mixture was heated
  2. temperatureat reflux for 6h
  3. temperatureThe mixture was cooled
  4. filtrationfiltered through celite
  5. concentrationthe filtrate was concentrated in vacuo
  6. customThe residue was purified by chromatography on silica

出典と根拠

ORDレコード
ord-5f701094615f4043b45cecee0d25df06
出典データセット
uspto-grants-1995_08
特許番号
US05444074

反応ノート

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