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Formamide → 8-(2,6-Dichlorobenzoylamino)-4-(2-formylhydrazino)quinoline

HRID 613566
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HRID 613566 반응식
[Cl:1][C:2]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:3]=1[C:4]([NH:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[CH:14][CH:13]=[C:12]2[NH:17][NH2:18])=[O:5].[CH:24](N)=[O:25]>C(O)=O>[Cl:1][C:2]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:3]=1[C:4]([NH:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[N:15]=[CH:14][CH:13]=[C:12]2[NH:17][NH:18][CH:24]=[O:25])=[O:5]
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참가 물질

4

반응물 2

HCID 713FormamideHCID 19592850HCID 19592850, 화합물

생성물 1

HCID 195927348-(2,6-Dichlorobenzoylamino)-4-(2-formylhydrazino)quinoline수율 83.3%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

To a solution of 8-(2,6-dichlorobenzoylamino)-4-hydrazinoquinoline (200 mg) in formic acid (4 ml) was added formamide (26 mg), and the mixture was stirred at ambient temperature for 3 hours. The solvent was azeotropically removed with toluene. The residue was diluted with ethyl acetate, washed with water and saturated aqueous sodium bicarbonate solution, dried over magnesium sulfate and concentrated in vacuo. The residual solid was treated with hot ethanol (2 ml), allowed to cool to ambient temperature, filtered and washed with ethanol to give 8-(2,6-dichlorobenzoylamino)-4-(2-formylhydrazino)quinoline (180 mg) as pale yellow crystal.

후처리

  1. customThe solvent was azeotropically removed with toluene
  2. additionThe residue was diluted with ethyl acetate
  3. washwashed with water and saturated aqueous sodium bicarbonate solution
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. additionThe residual solid was treated with hot ethanol (2 ml)
  7. temperatureto cool to ambient temperature
  8. filtrationfiltered
  9. washwashed with ethanol

출처 및 근거

ORD 기록
ord-465418af947342fa9aa5194a189f76fa
출처 데이터셋
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06008230

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