Sodium Hydroxide → 2-(2-Amino-phenoxy)-ethanol

HRID 1954662노트

반응식

HRID 1954662 반응식
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[N+:11]([O-])=O.Cl[Sn]Cl.[Sn].[OH-].[Na+]>Cl.O>[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH2:11]

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 24479Stannous ChlorideHCID 27370592-(2-Nitrophenoxy)ethanolHCID 5352426Tin atom

생성물 1

HCID 125388802-(2-Amino-phenoxy)-ethanol수율 80.6%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

반응 조건

온도
90 °C

실험 절차

8.9 g (48.59 mmol) 2-(2-hydroxyethoxy)nitrobenzene A2, 16.44 g (72.88 mmol) SnCl2. 2H2O and 17.3 g (145.77 mmol) tin were stirred in 30.84 ml aqueous HCl (30%) and 25 ml water at 90° C. for 8 hours. After cooling, the solution was treated with aqueous 5n sodium hydroxide solution and stirred for 3 hours at 90° C. The aqueous solution was subsequently decanted, wherein, upon cooling, the crude product crystallized out and was removed by suction. This crude product was then taken up in methanol, warmed and the suspension was filtered. The filtrate was then concentrated in vacuo. 6 g of light-brown crystals were obtained; yield 80%.

후처리

  1. temperatureAfter cooling
  2. customThe aqueous solution was subsequently decanted
  3. temperaturewherein, upon cooling
  4. customthe crude product crystallized out
  5. customwas removed by suction
  6. temperaturewarmed
  7. filtrationthe suspension was filtered
  8. concentrationThe filtrate was then concentrated in vacuo

출처 및 근거

ORD 기록
ord-a72711845d1344cf888d5e64c5a6d13f
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06124135

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