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Ammonium Chloride → (+/-)-3-(3-Aminophenyl)-5-(2,6-dichlorophenyl)-2-isoxazoline

HRID 2053388
ノート
印刷プレビュー

反応式

HRID 2053388 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH:9]1[O:13][N:12]=[C:11]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-])=O)[CH:15]=2)[CH2:10]1.[Cl-].[NH4+]>C(O)C.O.[Fe]>[NH2:20][C:16]1[CH:15]=[C:14]([C:11]2[CH2:10][CH:9]([C:3]3[C:4]([Cl:8])=[CH:5][CH:6]=[CH:7][C:2]=3[Cl:1])[O:13][N:12]=2)[CH:19]=[CH:18][CH:17]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 69221841(+/-)-5-(2,6-Dichlorophenyl)-3-(3-nitrophenyl)-2-isoxazoline

生成物 1

HCID 69222917(+/-)-3-(3-Aminophenyl)-5-(2,6-dichlorophenyl)-2-isoxazoline

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 19096565Water ethanol溶媒

反応条件

温度
80 °C

実験手順

Iron powder (99 mg, 1.78 mmol) was added into a suspension of (±)-5-(2,6-dichlorophenyl)-3-(3-nitrophenyl)-2-isoxazoline (100 mg, 0.297 mmol) in ethanol/water (2/1) under nitrogen. The mixture was stirred for 10 min, followed by the addition of ammonium chloride (32 mg, 0.594 mmol). The reaction was stirred for 20 min at room temperature, followed by heating at 80° C. for 1.5 h. The reaction mixture was cooled to room temperature and filtered through a plug of Celite. The filtrate was concentrated. The residue was dissolved in ethyl acetate and washed with aqueous sodium bicarbonate solution. The ethyl acetate layer was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by column chromatography on silica gel, eluting with 8:2 hexanes-ethyl acetate to provide the title compound as a light yellow solid.

後処理

  1. stirringThe reaction was stirred for 20 min at room temperature
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationfiltered through a plug of Celite
  4. concentrationThe filtrate was concentrated
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washwashed with aqueous sodium bicarbonate solution
  7. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe resulting residue was purified by column chromatography on silica gel
  11. washeluting with 8:2 hexanes-ethyl acetate

出典と根拠

ORDレコード
ord-6456801a2c2d40c28209e30cae4de906
出典データセット
uspto-grants-2008_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07326790B2

反応ノート

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