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Acetic Acid → HCID 20152418、化合物

HRID 4405
ノート
印刷プレビュー

反応式

HRID 4405 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[O:9][C:10]([CH3:25])=[C:11]([CH2:13][CH2:14][O:15][C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][CH:17]=2)[N:12]=1.C(O)(=O)C>O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[O:9][C:10]([CH3:25])=[C:11]([CH2:13][CH2:14][O:15][C:16]2[CH:17]=[CH:18][C:19]([NH2:22])=[CH:20][CH:21]=2)[N:12]=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

4

反応物 2

HCID 176Acetic AcidHCID 137139694-{2-[2-(2-Chlorophenyl)-5-methyl-4-oxazolyl]ethoxy}nitrobenzene

生成物 1

HCID 20152418HCID 20152418、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

Reduced iron (10.6 g) was added portionwise mixture of 4-{2-[2-(2-chlorophenyl)-5-methyl-4-oxazolyl]ethoxy}nitrobenzene (22.9 g), acetic acid (150 ml) and water (50 ml) at 70° C. After stirring at 80° C. for 2 hours, the insoluble matter was filtered off, and the filtrate was concentrated under reduced pressure. Water was added to the filtrate, and the aqueous mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4) and concentrated to give 4-{2-[2-(2-chlorophenyl)-5-methyl-4-oxazolyl]ethoxy}aniline as a crude oily material (20.5 g, 97.6%). NMR δppm in CDCl3 : 2.35(3H, s), 2.93(2H, t, J=7 Hz), 3.77(2H, s), 4.15(2H, t, J=7 Hz), 6.56(2H, d, J=9 Hz), 6.75(2H, d, J= 9 Hz), 7.2 to 7.5(3H, m), 7.9 (1H, m).

後処理

  1. filtrationthe insoluble matter was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionWater was added to the filtrate
  4. extractionthe aqueous mixture was extracted with ethyl acetate
  5. washThe ethyl acetate layer was washed with water
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-4df1147214394778b695246102bc2d3e
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04725610

反応ノート

読み込み中…

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