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

HRID 1372482노트

반응식

HRID 1372482 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3f3ceabebe694876b3ffc340dd9289b1
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157490B2

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