N-Iodosuccinimide → HCID 178494260, 화합물

HRID 473737노트

반응식

HRID 473737 반응식
[CH3:1][O:2][C:3]1[NH:4][CH:5]=[CH:6][C:7](=[O:9])[N:8]=1.C1C(=O)N([I:17])C(=O)C1>CN(C=O)C.O>[I:17][C:6]1[C:7](=[O:9])[N:8]=[C:3]([O:2][CH3:1])[NH:4][CH:5]=1

참가 물질

5

반응물 2

HCID 120273N-IodosuccinimideHCID 178494255HCID 178494255, 화합물

생성물 1

HCID 178494260HCID 178494260, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

2-Methoxypyrimidin-4(1H)-one (1.00 g, 7.93 mmol) and n-iodosuccinimide (3.57 g, 15.86 mmol) were mixed in DMF (8 mL) under a nitrogen atmosphere. The reaction mixture was stirred at 70° C. for 2.5 h. The reaction mixture was cooled to room temperature, diluted with water, and extracted with EtOAc (3×). The combined organic layers were washed with sat. sodium chloride, dried over magnesium sulfate, filtered, and concentrated. The resulting solid was suspended in DCM, filtered, and washed with DCM to give 5-iodo-2-methoxypyrimidin-4(1H)-one. MS (ESI, pos. ion) m/z: 252.9 (M+1).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionextracted with EtOAc (3×)
  3. washThe combined organic layers were washed with sat. sodium chloride
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. filtrationfiltered
  8. washwashed with DCM

출처 및 근거

ORD 기록
ord-4c8fc64b5fef4392bfa67c51e5d1a98c
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637500B2

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