Aniline → 1-(Phenylamino)butan-2-ol

HRID 4121

반응식

HRID 4121 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 140721971-(Phenylamino)butan-2-ol

시약·촉매·용매 2

HCID 962Water용매2회HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-81dc0c6c46c04f688c9e0a0ed9716418
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04723986

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