Sodium Azide → 4-Azido-8-fluoroquinoline

HRID 235047

反応式

HRID 235047 の反応式
Cl[C:2]1[C:11]2[C:6](=[C:7]([F:12])[CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][CH:3]=1.[N-:13]=[N+:14]=[N-:15].[Na+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.ClCCl.O>[N:13]([C:2]1[C:11]2[C:6](=[C:7]([F:12])[CH:8]=[CH:9][CH:10]=2)[N:5]=[CH:4][CH:3]=1)=[N+:14]=[N-:15]

参加物

6

反応物 2

HCID 33557Sodium AzideHCID 27365874-Chloro-8-fluoroquinoline

生成物 1

HCID 157905214-Azido-8-fluoroquinoline収率 93.2%

試薬・触媒・溶媒 3

HCID 74236Tetrabutylammonium Bromide触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2.08 g (0.0114 mol) of 4-chloro-8-fluoroquinoline, 1.12 g (0.0172 mol) of sodium azide, and 4.10 g ((0.0127 mol) of tetrabutyl ammonium bromide in 70 mL of dichloromethane and 25 mL of water was refluxed overnight. The layers were then separated and the organic layer was washed once with water, passed through phase separating paper, and concentrated to an oil, which was triturated with ether. The solid was filtered and the filtrate was concentrated to give 2.0 g of the title product.

後処理

  1. temperaturewas refluxed overnight
  2. customThe layers were then separated
  3. washthe organic layer was washed once with water
  4. customseparating paper
  5. concentrationconcentrated to an oil, which
  6. customwas triturated with ether
  7. filtrationThe solid was filtered
  8. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-276fd8bdc9a64e789f514668a6ca3727
出典データセット
uspto-grants-1997_01
特許番号
US05597836

関連ノート

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