1,1'-Carbonyldiimidazole → 6-Iodo-[1,2,4]triazolo[4,3-a]pyridin-3(2h)-one

HRID 1372482ノート

反応式

HRID 1372482 の反応式
[I:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][NH2:9])=[N:6][CH:7]=1.C1N=CN([C:15](N2C=NC=C2)=[O:16])C=1>ClCCl>[I:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:15](=[O:16])[NH:9][N:8]=2)[CH:7]=1

参加物

4

反応物 2

HCID 682631,1'-CarbonyldiimidazoleHCID 223971882-Hydrazinyl-5-iodopyridine

生成物 1

HCID 587793486-Iodo-[1,2,4]triazolo[4,3-a]pyridin-3(2h)-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 5-iodo-2-hydrazinopyridine (470 mg, 2 mmol) in dichloromethane (30 mL) was added a solution of N,N-carbonyldiimidazole (389 mg, 2.4 mmol) in 20 mL of dichloromethane. After stirring at room temperature for 2 h, the mixture was washed sequentially with water, 0.5N aqueous hydrochloric acid and saturated aqueous sodium bicarbonate solution. The organic phase was dried (magnesium sulfate) and concentrated under reduced pressure to afford the product. The resultant yellow crystals that precipitated from the aqueous phase upon standing overnight were collected and dried in vacuo to afford additional product. LC/MS 261.8 (M+1).

後処理

  1. washthe mixture was washed sequentially with water, 0.5N aqueous hydrochloric acid and saturated aqueous sodium bicarbonate solution
  2. dry with materialThe organic phase was dried (magnesium sulfate)
  3. concentrationconcentrated under reduced pressure
  4. customto afford the product
  5. customThe resultant yellow crystals that precipitated from the aqueous phase
  6. waitupon standing overnight
  7. customwere collected
  8. customdried in vacuo
  9. customto afford additional product

出典と根拠

ORDレコード
ord-3f3ceabebe694876b3ffc340dd9289b1
出典データセット
uspto-grants-2007_01
特許番号
US07157490B2

反応ノート

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