Benzoyl Peroxide → HCID 10910383、化合物

HRID 882148ノート

反応式

HRID 882148 の反応式
[C:1]([O:7][CH3:8])(=[O:6])/[C:2](=[CH:4]/[CH3:5])/[CH3:3].C1C(=O)N([Br:16])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:16][CH2:5]/[CH:4]=[C:2](\[CH3:3])/[C:1]([O:7][CH3:8])=[O:6]

参加物

5

反応物 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 53236522-Butenoic acid, 2-methyl-, methyl ester, (2E)-

生成物 1

HCID 10910383HCID 10910383、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

To a solution of methyl tiglate (2.00 g, 17.5 mmol) in CCl4 (8.76 mL) was added NBS (3.43 g, 19.3 mmol) and benzoyl peroxide (212 mg, 0.876 mmol). The reaction was heated to reflux for 3 hours, cooled and filtered through Celite using DCM to wash the filtrate. The reaction was concentrated in vacuo and then purified by silica chromatography using 1-15% EtOAc/hexane. The product was collected and concentrated in vacuo to afford the desired product as a colorless oil that was taken on to the next step without further purification.

後処理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 3 hours
  3. temperaturecooled
  4. filtrationfiltered through Celite
  5. washto wash the filtrate
  6. concentrationThe reaction was concentrated in vacuo
  7. custompurified by silica chromatography
  8. customThe product was collected
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-778fffb3877a40e49591b42828642c31
出典データセット
uspto-grants-2015_03
特許番号
US08993756B2

反応ノート

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