Benzylamine → N-(2-Methoxyphenyl)-2-[(phenylmethyl)amino]acetamide

HRID 728919ノート

反応式

HRID 728919 の反応式
[CH2:1]([NH2:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:10][C:11]([NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[O:20][CH3:21])=[O:12]>C(O)C>[CH3:21][O:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[NH:13][C:11](=[O:12])[CH2:10][NH:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

実験手順

To ethanol (100 mL) add benzylamine (35 g, 0.33 mol) and 2-chloro-N-(2-methoxyphenyl)acetamide (22 g, 0.11 mol). Stir and heat the reaction at 50° C. Monitor the progress of the reaction by thin-layer chromatography. Upon completion of the reaction remove the precipitate that has formed by suction filtration and discard. Evaporate the filtrate and partition the residue between ethyl acetate and 2N NaOH(aq). Separate the organic layer and dry it over Na2SO4. Remove the drying agent by filtration and remove the solvent in vacuo. Chromatograph the residue on silica gel (400 g) using hexane/EtOAc (3/1) as eluent to obtain the title compound.

後処理

  1. temperatureheat
  2. customthe reaction at 50° C
  3. customMonitor the progress of the reaction by thin-layer chromatography
  4. customUpon completion of the reaction remove the precipitate that
  5. customhas formed by suction filtration and discard
  6. customEvaporate the filtrate
  7. custompartition the residue between ethyl acetate and 2N NaOH(aq)
  8. customSeparate the organic layer
  9. dry with materialdry it over Na2SO4
  10. customRemove the drying agent
  11. filtrationby filtration
  12. customremove the solvent in vacuo

出典と根拠

ORDレコード
ord-1df82836c36e42c6a115b68dbe6395f8
出典データセット
uspto-grants-1991_09
特許番号
US05051422

反応ノート

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