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

HRID 1379018
ノート
印刷プレビュー

反応式

HRID 1379018 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 229090125-(4-Fluorophenyl)-4-(pyridin-4-yl)isoxazole収率 97.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d9f4dad64fab411d9359be414fae2925
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05670503

反応ノート

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