Aniline → 1-(Phenylamino)butan-2-ol

HRID 4121

反応式

HRID 4121 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O1CCOCC1.[O:14]1[CH:16]([CH2:17][CH3:18])[CH2:15]1.[F-].[K+]>O.C(Cl)Cl>[C:2]1([NH:1][CH2:15][CH:16]([OH:14])[CH2:17][CH3:18])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 6115AnilineHCID 78341,2-EpoxybutaneHCID 312751,4-DioxaneHCID 522689Potassium Fluoride

生成物 1

HCID 140721971-(Phenylamino)butan-2-ol

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

Aniline, (102.3 g, 1.1 mole) was added to 50 ml of dioxane, 108 g of 1,2-epoxy butane and 1 g of potassium fluoride in 25 ml of water. The mixture heated to reflux for 30 hours. The mixture was poured into water, taken up in 200 ml of methylene chloride, dried over anhydrous magnesium sulfate and stripped under vacuum. The residue was distilled under vacuum and the product, b.p. 98°-106° C. at 0.15 mm, weighed 94 g and was 97% pure by GLPC. It was characterized by IR and NMR.

後処理

  1. temperatureThe mixture heated
  2. temperatureto reflux for 30 hours
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe residue was distilled under vacuum

出典と根拠

ORDレコード
ord-81dc0c6c46c04f688c9e0a0ed9716418
出典データセット
uspto-grants-1988_02
特許番号
US04723986

関連ノート

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