Ethanolamine → 2-[(2-Hydroxyethyl)amino]-3-nitrobenzonitrile

HRID 419934ノート

反応式

HRID 419934 の反応式
Cl[C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[CH2:13]([CH2:15][NH2:16])[OH:14]>C(O)C>[OH:14][CH2:13][CH2:15][NH:16][C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5]

参加物

4

反応物 2

HCID 700EthanolamineHCID 217860112-Chloro-3-nitrobenzonitrile

生成物 1

HCID 114470952-[(2-Hydroxyethyl)amino]-3-nitrobenzonitrile収率 89%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-chloro-3-nitrobenzonitrile (74 g, 0.408 mol) is mixed with ethanol (370 ml) and ethanolamine (57 ml). The mixture is stirred for 16 hrs at room temperature. To complete the reaction, the mixture is refluxed for 2 hours. After cooling, the mixture is concentrated under vacuum; the product precipitates as a red solid. To eliminate the ethanolamine hydrochloride salt, the suspension is triturated with 500 ml of water and filtrated under vacuum. The solid is washed with ethanol and ether then dried to give the desired product (75 g, 89%).

後処理

  1. customthe reaction
  2. temperaturethe mixture is refluxed for 2 hours
  3. temperatureAfter cooling
  4. concentrationthe mixture is concentrated under vacuum
  5. customthe product precipitates as a red solid
  6. customthe suspension is triturated with 500 ml of water
  7. filtrationfiltrated under vacuum
  8. washThe solid is washed with ethanol and ether
  9. customthen dried

出典と根拠

ORDレコード
ord-4fe0a309a44c4f9aae3504079b335762
出典データセット
uspto-grants-2012_01
特許番号
US08093402B2

反応ノート

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