Dimethylformamide → 2-Iodo-3-(4-methoxy-benzyloxy)-pyridine

HRID 61900

반응식

HRID 61900 반응식
[I:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[CH:4][N:3]=1.C([O-])([O-])=O.[K+].[K+].CN(C=O)C.[CH3:20][O:21][C:22]1[CH:29]=[CH:28][C:25]([CH2:26]Cl)=[CH:24][CH:23]=1>O>[I:1][C:2]1[C:7]([O:8][CH2:26][C:25]2[CH:28]=[CH:29][C:22]([O:21][CH3:20])=[CH:23][CH:24]=2)=[CH:6][CH:5]=[CH:4][N:3]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 699934-Methyloxybenzyl chlorideHCID 971792-Iodopyridin-3-ol

생성물 1

HCID 866638312-Iodo-3-(4-methoxy-benzyloxy)-pyridine수율 27.2%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
45 °C

실험 절차

2-Iodo-pyridin-3-ol (50 mg, 0.226 mmol), K2CO3 (62 mg, 0.452 mmol) and DMF (2 ml) were added with para-methoxybenzyl chloride (46 μL, 0.339 mmol), and the mixture was stirred overnight at 45° C. The resultant was added with water, and then extracted with ethyl acetate. The organic layer was washed with saturated brine, and the resulting residues obtained after concentration under reduced pressure were purified by silica gel column (ethyl acetate/hexane) to obtain the title compound (21 mg, 27%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. customthe resulting residues obtained
  4. concentrationafter concentration under reduced pressure
  5. customwere purified by silica gel column (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-0db4a42840764726a8adfa1e8cbbc81b
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440922B2

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