Iodine → (5-Iodo-pyridin-2-yl)-methyl-amine

HRID 1350676

反応式

HRID 1350676 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.[I:9]I.C([O-])(O)=O.[Na+]>CC(O)=O.O>[I:9][C:6]1[CH:7]=[CH:8][C:3]([NH:2][CH3:1])=[N:4][CH:5]=1

参加物

6

反応物 3

HCID 807IodineHCID 207272-Pyridinamine, N-methyl-HCID 516892Sodium Bicarbonate

生成物 1

HCID 11253290(5-Iodo-pyridin-2-yl)-methyl-amine収率 24.9%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a solution of 2-methylaminopyridine (Aldrich; 1.00 g, 9.25 mmol) in 10 mL of 1:1 HOAc and water was added 2.35 g (9.25 mmol) of I2. The resulting brown solution was heated to 80° C. for 3 h. After cooling to room temperature, the mixture was neutralized with saturated NaHCO3 and extracted with Et2O. The extract was washed with water and brine, dried with MgSO4, filtered, and concentrated to provide 540 mg of (5-iodo-pyridin-2-yl)-methyl-amine.

後処理

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with Et2O
  3. washThe extract was washed with water and brine
  4. dry with materialdried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-096fabc787d84b3ebc1428aa1af0c299
出典データセット
uspto-grants-2007_05
特許番号
US07214802B2

関連ノート

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