Benzoyl Peroxide → HCID 68428666、化合物

HRID 642315ノート

反応式

HRID 642315 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[S:9][C:10]=1[CH3:11])=[O:5])[CH3:2].[Br:18]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[C:8]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[S:9][C:10]=1[CH2:11][Br:18])=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 150939465-Methyl-2-phenyl-thiazole-4-carboxylic acid ethyl ester

生成物 1

HCID 68428666HCID 68428666、化合物収率 108.9%

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

A mixture of 5-methyl-2-phenyl-thiazole-4-carboxylic acid ethyl ester (7.76 g, 0.03 mol), N-bromosuccinimide (5.87 g, 0.03 mol) and benzoyl peroxide (761 mg, 3.30 mmol) in carbon tetrachloride (130 mL) was refluxed for 16 h before it was cooled to room temperature and partitioned between dichloromethane and water. The organic layer was washed with saturated aqueous sodium bicarbonate solution, brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound as a yellow oil (10.66 g); MS: (+) m/z 325.93, 328.00 (M+1, 79Br/81Br).

後処理

  1. temperaturewas refluxed for 16 h before it
  2. custompartitioned between dichloromethane and water
  3. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution, brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-437e0fd0ddaa44488157803f224918b5
出典データセット
uspto-grants-2010_04
特許番号
US07696223B2

反応ノート

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