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

HRID 61900

反応式

HRID 61900 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
45 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-0db4a42840764726a8adfa1e8cbbc81b
出典データセット
uspto-grants-2016_09
特許番号
US09440922B2

関連ノート

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