Benzoyl Peroxide → HCID 10910383, 화합물

HRID 882148노트

반응식

HRID 882148 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 10910383HCID 10910383, 화합물

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-778fffb3877a40e49591b42828642c31
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993756B2

반응 노트

불러오는 중…