Azobisisobutyronitrile → 1-(Bromomethyl)-2-(dibromomethyl)naphthalene

HRID 2296591노트

반응식

HRID 2296591 반응식
[Br:1][CH2:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][C:4]=1[CH2:13][Br:14].[Br:15]N1C(=O)CCC1=O.N(C(C)(C)C#N)=NC(C)(C)C#N>C(Cl)(Cl)(Cl)Cl>[Br:1][CH2:2][C:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[CH:6]=[CH:5][C:4]=1[CH:13]([Br:15])[Br:14]

참가 물질

5

반응물 3

HCID 6547AzobisisobutyronitrileHCID 67184N-bromobutanimideHCID 34035511,2-Bis(bromomethyl)naphthalene

생성물 1

HCID 123671501-(Bromomethyl)-2-(dibromomethyl)naphthalene수율 64%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

반응 조건

온도
100 °C

실험 절차

In 150 ml of carbon tetrachloride, 20 g (64 mmole) of 1,2-bis(bromomethyl)naphthalene and 23 g (130 mmole) of N-bromosuccinimide were suspended. To the obtained suspension, 1.1 g (6.7 mmole) of 2,2′-azobis(isobutyronitrile) was added and the mixture was vigorously stirred at 100° C. for 2 hours. After the reaction was completed, the reaction mixture was filtered and the residue was washed with 150 ml of dichloromethane. The filtrate and the washing were combined. The combined solution was treated by the column chromatography (silica gel/dichloromethane) without additional treatments and 16 g (the yield: 64%) of a white solid of 1-(bromomethyl)-2-(dibromomethyl)naphthalene was obtained.

후처리

  1. filtrationthe reaction mixture was filtered
  2. washthe residue was washed with 150 ml of dichloromethane
  3. additionThe combined solution was treated by the column chromatography (silica gel/dichloromethane) without additional treatments and 16 g (the yield: 64%) of a white solid of 1-(bromomethyl)-2-(dibromomethyl)naphthalene
  4. customwas obtained

출처 및 근거

ORD 기록
ord-26ee7c345b06443cb25915c9be1fb57a
출처 데이터셋
uspto-grants-2002_12
특허 번호
US06489046B1

반응 노트

불러오는 중…