Isoquinoline → 2-Aminoisoquinolinium Iodide

HRID 336980ノート

反応式

HRID 336980 の反応式
[NH2:1]OS(O)(=O)=O.[CH:7]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:10]=[CH:9][N:8]=1.C(=O)([O-])[O-].[K+].[K+].[IH:23]>O>[I-:23].[NH2:1][N+:8]1[CH:9]=[CH:10][C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:7]=1

参加物

6

反応物 4

HCID 8405IsoquinolineHCID 11430Potassium CarbonateHCID 24841Hydrogen iodideHCID 76284hydroxylamine-O-sulfonic acid

生成物 1

HCID 108586012-Aminoisoquinolinium Iodide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of hydroxylamine-O-sulfonic acid (2) (2 g, 1 equiv.), water (10 mL) and isoquinoline (1) (6.3 mL, 3 equiv.) was heated at 90° C. for 2-3 h. Potassium carbonate (2.44 g, 1 equiv.) was added, and the water was evaporated. Ethanol (20-30 mL) was added to the solid residue, and insoluble potassium sulfate was filtered out. Hydroiodic acid (57%-67%, 1.34 mL, 1 equiv.) was added to the filtrate, and the resulting solution was placed in a freezer. The precipitate was filtered out, washed with ethanol, and dried in vacuo. Isolated products were used as such in further reactions. Yield of the product was 1.78 g.

後処理

  1. customthe water was evaporated
  2. additionEthanol (20-30 mL) was added to the solid residue, and insoluble potassium sulfate
  3. filtrationwas filtered out
  4. filtrationThe precipitate was filtered out
  5. washwashed with ethanol
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-99d1ba09ac324ed69b0ec79c47ada600
出典データセット
uspto-grants-2014_11
特許番号
US08889713B1

反応ノート

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