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

HRID 1982160ノート

反応式

HRID 1982160 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0fe54f9a9f9748aaa1bece183eec0f55
出典データセット
uspto-grants-1986_06
特許番号
US04595689

反応ノート

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