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N-bromobutanimide → 1-Bromo-6-bromomethyl-2,3,4,5-tetramethoxybenzene

HRID 2268438
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HRID 2268438 반응식
[Br:1][C:2]1[C:7]([CH3:8])=[C:6]([O:9][CH3:10])[C:5]([O:11][CH3:12])=[C:4]([O:13][CH3:14])[C:3]=1[O:15][CH3:16].[Br:17]N1C(=O)CCC1=O>CC(N=NC(C#N)(C)C)(C#N)C.C(OCC)(=O)C>[Br:1][C:2]1[C:7]([CH2:8][Br:17])=[C:6]([O:9][CH3:10])[C:5]([O:11][CH3:12])=[C:4]([O:13][CH3:14])[C:3]=1[O:15][CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 125607691-Bromo-2,3,4,5-tetramethoxy-6-methylbenzene

생성물 1

HCID 183486201-Bromo-6-bromomethyl-2,3,4,5-tetramethoxybenzene수율 99.5%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 8857Ethyl Acetate용매

실험 절차

An ethyl acetate (300 ml) solution of 1-bromo-2,3,4,5-tetramethoxy-6-methylbenzene (49.5 g, 0.170 mols), N-bromosuccinimide (31.8 g, 0.179 mols) and AIBN (558 mg, 3.40 mmols) was heated under reflux for 1 hour. The reaction mixture was concentrated in vacuo, and then diluted with hexane. The resulting crystals were separated by filtration, and the filtrate was concentrated to obtain the entitled compound (62.6 g) as an oil.

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후처리

  1. temperatureunder reflux for 1 hour
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. additiondiluted with hexane
  4. customThe resulting crystals were separated by filtration
  5. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-5e97f78620604b55a49a76458f60ea52
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06326369B1

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