Hydrazine hydrate (1:1) → HCID 10199104, 화합물

HRID 395921노트

반응식

HRID 395921 반응식
O.[NH2:2][NH2:3].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11](=O)[C:12]#[C:13][C:14]2[S:15][CH:16]=[CH:17][CH:18]=2)=[CH:7][CH:6]=1>C(O)C.C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[C:13]([C:14]3[S:15][CH:16]=[CH:17][CH:18]=3)[NH:3][N:2]=2)=[CH:7][CH:6]=1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 13360982HCID 13360982, 화합물

생성물 1

HCID 10199104HCID 10199104, 화합물수율 80%

시약·촉매·용매 2

HCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)촉매HCID 702Ethanol용매

실험 절차

Hydrazine hydrate (228 mg, 4.6 mM) and pyridinium p-toluenesulfonate (50 mg) were added to a solution of 1-(4-chlorophenyl)-3-(2-thienyl)-2-propyn-1-one (750 mg, 3.0 mM) in ethanol (30 ml), and this mixture was heated under reflux for 2 hours. After the mixture was allowed to cool to room temperature, the solvent was distilled off under reduced pressure, and the resulting residue was dissolved in ethyl acetate (50 ml). This solution was washed with a saturated aqueous solution of sodium hydrogen carbonate and a saturated aqueous solution of sodium chloride, and dried over magnesium sulfate. Thereafter, the solvent was distilled off under reduced pressure to obtain 634 mg of 3-(4-chlorophenyl)-5-(2-thienyl)-1H-pyrazole, m.p. 217° C., in an 80% yield.

후처리

  1. temperaturethis mixture was heated
  2. temperatureunder reflux for 2 hours
  3. distillationthe solvent was distilled off under reduced pressure
  4. dissolutionthe resulting residue was dissolved in ethyl acetate (50 ml)
  5. washThis solution was washed with a saturated aqueous solution of sodium hydrogen carbonate
  6. dry with materiala saturated aqueous solution of sodium chloride, and dried over magnesium sulfate
  7. distillationThereafter, the solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-16672854e8c643fb87fb9437dbc1d43f
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06605730B2

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