N-bromobutanimide → 4-(broMoMethyl)-2-broMoanisole

HRID 491412노트

반응식

HRID 491412 반응식
[Br:1][C:2]1[CH:7]=[C:6]([CH3:8])[CH:5]=[CH:4][C:3]=1[O:9][CH3:10].[Br:11]N1C(=O)CCC1=O>CC(N=NC(C#N)(C)C)(C#N)C>[Br:1][C:2]1[CH:7]=[C:6]([CH:5]=[CH:4][C:3]=1[O:9][CH3:10])[CH2:8][Br:11]

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 891432-Bromo-4-methylanisole

생성물 1

HCID 112774624-(broMoMethyl)-2-broMoanisole수율 100%

시약·촉매·용매 1

HCID 6547Azobisisobutyronitrile촉매

실험 절차

2-Bromo-4-methyl anisole 14 (2.2 mL, 14.9 mmol) was dissolved in dichlomethane (30 mL) and N-bromosuccinimide (3.75 g, 16.4 mmol) was added followed by AIBN (26.0 mg). The reaction was heated to reflux for 19 hrs., then cooled to room temperature and the precipitate was filtered off. The filtrate was diluted with dichloromethane and washed with 0.5 M aqueous sodium bicarbonate, followed by water. The organic mixture was dried over sodium sulfate, filtered and concentrated under vacuum to yield 15 (4.16 g, 100%). The benzyl bromide was used as the crude material without further purification.

후처리

  1. additionwas added
  2. temperatureThe reaction was heated
  3. temperatureto reflux for 19 hrs
  4. filtrationthe precipitate was filtered off
  5. additionThe filtrate was diluted with dichloromethane
  6. washwashed with 0.5 M aqueous sodium bicarbonate
  7. dry with materialThe organic mixture was dried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-5109376a568e483292ffa4820f2aa5f8
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07531544B2

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