Water → Ethyl 2-(3,6-dichloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionate

HRID 1067597노트

반응식

HRID 1067597 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[C:9]([C:11]([CH3:18])([CH3:17])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[N:10]=2)[N:7]=1.[Cl:19]N1C(=O)CCC1=O.O>C(OCC)(=O)C>[Cl:19][C:8]1[N:6]2[N:7]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]2=[N:10][C:9]=1[C:11]([CH3:17])([CH3:18])[C:12]([O:14][CH2:15][CH3:16])=[O:13]

참가 물질

5

반응물 3

HCID 962WaterHCID 31398ChlorosuccinimideHCID 11043751Ethyl 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropanoate

생성물 1

HCID 22989216Ethyl 2-(3,6-dichloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionate수율 97.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

4.07 g of ethyl 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionate was suspended in 60 ml of ethyl acetate; 2.13 g of N-chlorosuccinimide was added, followed by thermal refluxing for 4 hours. After cooling, water was added, followed by extraction with ethyl acetate; the extract was washed with saturated saline and dried with magnesium sulfate. The dry product was concentrated under reduced pressure; the residue was subjected to silica gel column chromatography and eluted with hexane:ethyl acetate (5:1). The desired fraction was collected and concentrated under reduced pressure to yield 4.48 g of the title compound.

후처리

  1. customrefluxing for 4 hours
  2. temperatureAfter cooling
  3. extractionfollowed by extraction with ethyl acetate
  4. washthe extract was washed with saturated saline
  5. dry with materialdried with magnesium sulfate
  6. concentrationThe dry product was concentrated under reduced pressure
  7. washeluted with hexane:ethyl acetate (5:1)
  8. customThe desired fraction was collected
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-af83afebb6d5400cbd2686ba8a0a1beb
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06248740B1

반응 노트

불러오는 중…