Methyl iodide → 4-(8-Bromodibenz[b,f]oxepin-10-yl)-1-methylpyridinium iodide

HRID 1982160노트

반응식

HRID 1982160 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[CH:8]=[C:7]([C:16]3[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=3)[C:6]=2[CH:22]=1.[CH3:23][I:24]>C(#N)C>[I-:24].[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[CH:8]=[C:7]([C:16]3[CH:17]=[CH:18][N+:19]([CH3:23])=[CH:20][CH:21]=3)[C:6]=2[CH:22]=1

참가 물질

4

반응물 2

HCID 6328Methyl iodideHCID 136086134-(8-Bromodibenz[b,f]oxepin-10-yl)pyridine

생성물 1

HCID 233174974-(8-Bromodibenz[b,f]oxepin-10-yl)-1-methylpyridinium iodide

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 4-(8-bromodibenz[b,f]oxepin-10-yl)pyridine (2.0 g) in acetonitrile (30 ml) containing methyl iodide (1.1 ml) was stirred under reflux in an argon atmosphere for ninety minutes. During this time the starting material gradually dissolved and a yellow solid began to precipitate from solution. The mixture was cooled to -10° and the solids were collected by filtration and were washed in turn with cold acetonitrile and ether to give 2.7 g of 4-(8-bromo-dibenz[b,f]oxepin-10-yl)-1-methylpyridinium iodide.

후처리

  1. temperatureunder reflux in an argon atmosphere for ninety minutes
  2. dissolutionDuring this time the starting material gradually dissolved
  3. customto precipitate from solution
  4. temperatureThe mixture was cooled to -10°
  5. filtrationthe solids were collected by filtration
  6. washwere washed in turn with cold acetonitrile and ether

출처 및 근거

ORD 기록
ord-0fe54f9a9f9748aaa1bece183eec0f55
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04595689

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