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

HRID 603104노트

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HRID 603104 반응식
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]

참가 물질

4

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b006bfee7b324cbe8f48d7abc168c173
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07906654B2

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