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

HRID 1350676

반응식

HRID 1350676 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-096fabc787d84b3ebc1428aa1af0c299
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214802B2

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