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1,4-Dioxane → HCID 15766695, 화합물

HRID 1707584
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HRID 1707584 반응식
O1CCOCC1.[F:7][C:8]([F:24])([F:23])[C:9]1[C:10]([S:15]([NH:18][C:19](=[O:22])OC)(=[O:17])=[O:16])=[N:11][CH:12]=[CH:13][CH:14]=1.[CH3:25][C:26]1[CH2:30][C:29]([CH3:37])([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[NH:28][N:27]=1>N1C=CC=CC=1>[F:23][C:8]([F:7])([F:24])[C:9]1[C:10]([S:15]([NH:18][C:19]([N:28]2[C:29]([CH3:37])([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)[CH2:30][C:26]([CH3:25])=[N:27]2)=[O:22])(=[O:16])=[O:17])=[N:11][CH:12]=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 312751,4-DioxaneHCID 15766693HCID 15766693, 화합물HCID 18961696HCID 18961696, 화합물

생성물 1

HCID 15766695HCID 15766695, 화합물수율 86%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A dry dioxane (10 ml) solution containing methyl N-(3-trifluoromethylpyridine-2-sulfonyl)carbamate (0.43 g, 1.5 mmol), 3,5-dimethyl-5-phenyl-2-pyrazoline (0.52 g, 3.0 mmol) and pyridine (0.45 g) was refluxed under heating and stirring for one-hour. After cooling the mixture, the solvent was distilled off under reduced pressure, and the residue was stirred together with ethyl ether. Precipitated crystals were collected by filtration and then thoroughly washed with ethyl ether, and the crystals were suspended in 20 ml of water. Then, the pH was adjusted to a level of from 1 to 2 with concentrated hydrochloric acid, and the suspension was stirred at room temperature for 5 minutes. Crystals were collected by filtration, thoroughly washed with water and then with ethyl ether and dried to obtain 0.55 g of desired 1-(3-trifluoromethylpyridine-2-sulfonylcarbamoyl)-3,5-dimethyl-5-phenyl-2-pyrazoline. Melting point: 152°-153° C.

후처리

  1. temperaturewas refluxed
  2. temperatureunder heating
  3. temperatureAfter cooling the mixture
  4. distillationthe solvent was distilled off under reduced pressure
  5. stirringthe residue was stirred together with ethyl ether
  6. customPrecipitated crystals
  7. filtrationwere collected by filtration
  8. washthoroughly washed with ethyl ether
  9. stirringthe suspension was stirred at room temperature for 5 minutes
  10. filtrationCrystals were collected by filtration
  11. washthoroughly washed with water
  12. dry with materialwith ethyl ether and dried

출처 및 근거

ORD 기록
ord-6187d755edf140daa7e340e6972f7ddd
출처 데이터셋
uspto-grants-1994_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05354731

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