Potassium Hydroxide → HCID 13958990, 화합물

HRID 255855노트

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HRID 255855 반응식
Cl.N[OH:3].[OH-].[K+].[N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([C:16]#[N:17])=[CH:8][N:7]=1>C(O)C>[N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:9]([C:16]([NH2:17])=[O:3])=[CH:8][N:7]=1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 5932574-Cinnolinecarbonitrile

생성물 1

HCID 13958990HCID 13958990, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

0.76 g of hydroxylamine hydrochloride was added to a stirred solution of 0.72 g of 85% aqueous potassium hydroxide in 25 ml of absolute ethanol at room temperature. The mixture was stirred at room temperature for 20 minutes, then 1.55 g of 27C was added and the mixture was heated at reflux for 3 hours, held overnight at room temperature, and filtered. The filtrate was stripped of solvent to give a dark oil, from which a yellow solid precipitated on standing. The solid was separated, and stirred in hot ethyl acetate. The resulting mixture was filtered, the solvent was stripped from the filtrate and the residue was recrystallized from ethanol to give 27, as a yellow solid, m.p.: 223° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 3 hours
  3. waitheld overnight at room temperature
  4. filtrationfiltered
  5. customto give a dark oil
  6. customfrom which a yellow solid precipitated
  7. customThe solid was separated
  8. stirringstirred in hot ethyl acetate
  9. filtrationThe resulting mixture was filtered
  10. customthe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-13437b95c4ef4531a91bcb2765312a37
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04699651

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