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N-Iodosuccinimide → HCID 59654182, 화합물

HRID 1784470
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HRID 1784470 반응식
[Cl:1][CH2:2][C:3]1[N:4]=[C:5]2[CH:13]=[CH:12][CH:11]=[CH:10][N:6]2[C:7](=[O:9])[CH:8]=1.[I:14]N1C(=O)CCC1=O>C(#N)C>[Cl:1][CH2:2][C:3]1[N:4]=[C:5]2[CH:13]=[CH:12][CH:11]=[CH:10][N:6]2[C:7](=[O:9])[C:8]=1[I:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 120273N-IodosuccinimideHCID 51550272-(chloromethyl)-4H-pyrido(1,2-a)pyrimidin-4-one

생성물 1

HCID 59654182HCID 59654182, 화합물수율 83%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
80 °C

실험 절차

A mixture of 21.9 g (112.5 mmol) of the product from Step 1 (11) and 38.9 g (168.8 mmol) of N-iodosuccinimide in 660 mL of acetonitrile was stirred at 80° C. under nitrogen for 16 hours. The reaction mixture was then allowed to cool to ambient temperature and the acetonitrile was removed in vacuo. The resulting solid was washed with water, saturated Na2O3S2, saturated NaHCO3, brine, and filtered. Drying under reduced pressure at 40° C. overnight yielded 29.8 g (92.9 mmol, 83%) of 2-(chloromethyl)-3-iodo-4H-pyrido[1,2-a]pyrimidin-4-one (12) as a light brown solid.

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후처리

  1. temperatureto cool to ambient temperature
  2. customthe acetonitrile was removed in vacuo
  3. washThe resulting solid was washed with water, saturated Na2O3S2, saturated NaHCO3, brine
  4. filtrationfiltered
  5. customDrying under reduced pressure at 40° C. overnight

출처 및 근거

ORD 기록
ord-1ca7ce72ffee42aaba2034928fa59554
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07504405B2

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