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

HRID 2105104ノート

反応式

HRID 2105104 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-220eb2f3f15644d783f300d6b4e22aea
出典データセット
uspto-grants-2009_08
特許番号
US07579140B2

反応ノート

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