3-Fluoroaniline → 3-Fluoro-4-thiocyanatoaniline

HRID 2305646ノート

反応式

HRID 2305646 の反応式
BrN1C(=O)CCC1=O.[S-:9][C:10]#[N:11].[K+].[F:13][C:14]1[CH:15]=[C:16]([CH:18]=[CH:19][CH:20]=1)[NH2:17]>CO>[F:13][C:14]1[CH:15]=[C:16]([CH:18]=[CH:19][C:20]=1[S:9][C:10]#[N:11])[NH2:17]

参加物

5

反応物 3

HCID 97423-FluoroanilineHCID 67184N-bromobutanimideHCID 516872Potassium thiocyanate

生成物 1

HCID 222450793-Fluoro-4-thiocyanatoaniline

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

N-Bromosuccinimide (1.76 g, 9.89 mmol) and potassium thiocyanate (1.75 g, 18.0 mmol) in methanol (30 ml) were stirred for 15 minutes at room temperature. The reaction mixture was cooled to 0° C., and 3-fluoroaniline (1.00 g, 9.0 mmol) was added dropwise. The mixture was stirred at 0° C. for 2 h. Solvent was removed under vacuum, and the residue was washed with dichloromethane. The mixture was filtered to remove succinimide by-product, and the solution was washed with water, brine, and dried (MgSO4). Solvent was removed under vacuum to afford the desired product as a colorless oil. Yield 1.45 g (96%).

後処理

  1. customSolvent was removed under vacuum
  2. washthe residue was washed with dichloromethane
  3. filtrationThe mixture was filtered
  4. customto remove succinimide by-product
  5. washthe solution was washed with water, brine
  6. dry with materialdried (MgSO4)
  7. customSolvent was removed under vacuum

出典と根拠

ORDレコード
ord-1525ca33e4fa43e0a2dbfc004834101b
出典データセット
uspto-grants-2002_08
特許番号
US06441005B1

反応ノート

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