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Hydroxyamine hydrochloride → 5-(4-Fluorophenyl)-4-(pyridin-4-yl)isoxazole

HRID 1379018
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HRID 1379018 반응식
C[N:2](C)[CH:3]=[C:4]([C:14]1[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=1)[C:5]([C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][CH:8]=1)=[O:6].Cl.NO>C(O)C>[F:13][C:10]1[CH:11]=[CH:12][C:7]([C:5]2[O:6][N:2]=[CH:3][C:4]=2[C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 545188383-(Dimethylamino)-1-(4-fluorophenyl)-2-(pyridin-4-yl)prop-2-en-1-one

생성물 1

HCID 229090125-(4-Fluorophenyl)-4-(pyridin-4-yl)isoxazole수율 97.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 3-dimethylamino-1-(4-fluorophenyl)-2-(pyridin-4-yl)-2-propen-1-one (6.15 g) and hydroxylamine hydrochloride (4.75 g) in dry ethanol (40 ml) was refluxed for 20 minutes. The mixture was cooled and concentrated in vacuo. The residue was dissolved in dilute hydrochloric acid and then treated with an aqueous saturated sodium bicarbonate solution. The precipitates were collected by filtration, washed with water, and dried to give 5-(4-fluorophenyl)-4-(pyridin-4-yl)isoxazole (5.35 g).

후처리

  1. temperaturewas refluxed for 20 minutes
  2. temperatureThe mixture was cooled
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in dilute hydrochloric acid
  5. additiontreated with an aqueous saturated sodium bicarbonate solution
  6. filtrationThe precipitates were collected by filtration
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-d9f4dad64fab411d9359be414fae2925
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05670503

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