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

HRID 611761ノート

反応式

HRID 611761 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 125388802-(2-Amino-phenoxy)-ethanol収率 80.6%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-99afbdbf43ac4dd394936721c3dae138
出典データセット
uspto-grants-1999_12
特許番号
US06001999

反応ノート

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