Isoquinoline → 2-Aminoisoquinolinium Iodide

HRID 1036640

反応式

HRID 1036640 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-f8ce45c2a6ab4a57bf8d7f94db905dd5
出典データセット
uspto-grants-2013_10
特許番号
US08546426B2

関連ノート

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