Hydrogen Bromide → 1,2,3,4-Tetrahydroquinoxalin-5-amine

HRID 1082052ノート

反応式

HRID 1082052 の反応式
Cl.Cl.[NH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH2:10])[C:5]=1[NH:11][CH2:12][CH2:13]O.Br>>[NH:3]1[C:4]2[CH:9]=[CH:8][CH:7]=[C:6]([NH2:10])[C:5]=2[NH:11][CH2:12][CH2:13]1

参加物

3

反応物 2

HCID 260Hydrogen BromideHCID 23362031HCID 23362031、化合物

生成物 1

HCID 233620291,2,3,4-Tetrahydroquinoxalin-5-amine

反応条件

温度
-20 °C

実験手順

25 g (0.104 mol) of 2-[(2,6-diaminophenyl)amino]ethanol dihydrochloride are heated at 160° C. for 3 hours in 300 ml of a 62% hydrobromic acid solution. The reaction mixture is cooled to -20° C. until crystallization takes place and the precipitate obtained is dried, under nitrogen, with a mixture of methanol and ether. It is taken up in water, the pH is adjusted to alkaline with a concentrated sodium hydroxide solution and extraction is carried out with a dichloromethane/ether (50/50) mixture. Drying and evaporation are carried out.

後処理

  1. customthe precipitate obtained
  2. dry with materialis dried, under nitrogen, with a mixture of methanol and ether
  3. extractionto alkaline with a concentrated sodium hydroxide solution and extraction
  4. customDrying
  5. customevaporation

出典と根拠

ORDレコード
ord-e1702f8fc6cf4d32b294615ffdec5b23
出典データセット
uspto-grants-1996_12
特許番号
US05589476

反応ノート

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