2-Chloroethanol → 2-((4-Amino-2-chloro-5-nitrophenyl)amino)ethanol

HRID 1282962

反応式

HRID 1282962 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([NH2:9])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11].[CH2:13](Cl)[CH2:14][OH:15].[OH-].[Na+]>O>[NH2:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([NH:9][CH2:13][CH2:14][OH:15])=[CH:4][C:3]=1[N+:10]([O-:12])=[O:11]

参加物

5

反応物 3

HCID 342-ChloroethanolHCID 14798Sodium HydroxideHCID 54842901,4-Benzenediamine, 2-chloro-5-nitro-

生成物 1

HCID 54902712-((4-Amino-2-chloro-5-nitrophenyl)amino)ethanol

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

18.7 g (0.1 mole) of 1,4-diamino-2-nitro-5-chlorobenzene were dissolved in 20 ml methylglycol and 12 g ethylenechlorohydrin (1.5 mole) and the solution then heated on a bath having a temperature of 120°C. 6.6 g of sodium hydroxide dissolved in 60 ml water were then slowly added dropwise over a period of 3 hours. Heating was then continued for 1 hour whereupon a chromatographic check wss made to ascertain whether most or all of the starting compound had been reacted. After cooling the mass was diluted with water and the precipitated hydroxyethylated compound was removed by suction. Recrystallation was effected from water and thereafter from a 20% acetic acid. Yield: 4.5 g; m.p.: 130°-131°C. Analysis: C8H10ClO3N3

後処理

  1. customa temperature of 120°C
  2. additionwere then slowly added dropwise over a period of 3 hours
  3. temperatureHeating
  4. customhad been reacted
  5. temperatureAfter cooling the mass
  6. customthe precipitated hydroxyethylated compound was removed by suction

出典と根拠

ORDレコード
ord-7dbc80d2dfcb4972b48b3f9643edad35
出典データセット
uspto-grants-1976_08
特許番号
US03973900

関連ノート

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