4-Methoxy-2-pyrimidinamine → 5-Iodo-4-methoxypyrimidin-2-amine

HRID 881422

반응식

HRID 881422 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][N:6]=[C:5]([NH2:9])[N:4]=1.[I:10]N1C(=O)CCC1=O>C(O)(=O)C>[I:10][C:8]1[C:3]([O:2][CH3:1])=[N:4][C:5]([NH2:9])=[N:6][CH:7]=1

참가 물질

4

반응물 2

HCID 674284-Methoxy-2-pyrimidinamineHCID 120273N-Iodosuccinimide

생성물 1

HCID 534854215-Iodo-4-methoxypyrimidin-2-amine

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

To a solution of 4-methoxy-pyrimidin-2-ylamine (405 mg) in acetic acid (10 mL) was added N-iodosuccinimide (950 mg) and the mixture was heated at 80° C. for 4 h. After cooling to room temperature, the reaction was quenched with 5% aqueous sodium thiosulphate solution (20 mL) and the solvent removed in vacuo. The product was then extracted into dicholoromethane (3×20 mL) and the combined organics were washed with brine (40 mL), dried (MgSO4) and reduced in vacuo to give 5-iodo-4-methoxy-pyrimidin-2-ylamine as a white solid.

후처리

  1. temperatureAfter cooling to room temperature
  2. customthe reaction was quenched with 5% aqueous sodium thiosulphate solution (20 mL)
  3. customthe solvent removed in vacuo
  4. extractionThe product was then extracted into dicholoromethane (3×20 mL)
  5. washthe combined organics were washed with brine (40 mL)
  6. dry with materialdried (MgSO4)

출처 및 근거

ORD 기록
ord-cb62bd9cb2924ba1bb504b61235ce3c8
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08993563B2

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