Methyl iodide → Quinolinium, 1,2-dimethyl-6-nitro-, iodide

HRID 389244

反応式

HRID 389244 の反応式
[CH3:1][C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([N+:12]([O-:14])=[O:13])[CH:8]=2)[N:3]=1.[I:15][CH3:16]>C(#N)C>[I-:15].[CH3:16][N+:3]1[C:4]2[C:9](=[CH:8][C:7]([N+:12]([O-:14])=[O:13])=[CH:6][CH:5]=2)[CH:10]=[CH:11][C:2]=1[CH3:1]

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 691722-Methyl-6-nitroquinoline

生成物 1

HCID 12252537Quinolinium, 1,2-dimethyl-6-nitro-, iodide収率 16.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2-Methyl-6-nitroquinoline (0.5 g, 2.66 mmol) and iodomethane (1 ml, 16 mmol) were heated together in acetonitrile (10 ml) at reflux for 48 hrs. The mixture was cooled to room temperature and a grey material crystallised out of solution and was filtered off. This was shown to be starting material. The filtrate was diluted with ethyl acetate (200 ml) to give a yellow/green precipitate. The product was filtered off, washed with ethyl acetate and then dried under vacuum. The product was obtained as a yellow/green solid (147 mg, 16.8%).

後処理

  1. temperatureat reflux for 48 hrs
  2. customa grey material crystallised out of solution
  3. filtrationwas filtered off
  4. additionThe filtrate was diluted with ethyl acetate (200 ml)
  5. customto give a yellow/green precipitate
  6. filtrationThe product was filtered off
  7. washwashed with ethyl acetate
  8. customdried under vacuum

出典と根拠

ORDレコード
ord-2e1642e27f364759a8acb8c27486709e
出典データセット
uspto-grants-2013_02
特許番号
US08378120B2

関連ノート

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