Zytron → HCID 86624412、化合物

HRID 910761

反応式

HRID 910761 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C@@H:9]([NH2:11])[CH3:10])=[CH:5][CH:4]=1.CC(NP(OC1C=CC(Cl)=CC=1Cl)(OC)=S)C.[CH2:29]=[C:30]1[O:33][C:32](=[O:34])[CH2:31]1>ClCCl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C@@H:9]([NH:11][C:32](=[O:34])[CH2:31][C:30](=[O:33])[CH3:29])[CH3:10])=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 9299ZytronHCID 12661DiketeneHCID 793467(S)-1-(4-Methoxyphenyl)ethylamine

生成物 1

HCID 86624412HCID 86624412、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
20 °C

実験手順

To a solution of (S)-1-(4-methoxy-phenyl)-ethylamine (25 g) in dichloromethane (60 mL) was added TEA (20 g) and DMPA (200 mg). Then a solution of 4-methylene-oxetan-2-one (16.7 g) in dichloromethane (60 ml) was added over a period of 30 minutes and then stirred at 20° C. for 18 h. The mixture was washed with 1M HCl, aq. NaHCO3 and aq. NaCl. The organic layer was dried (MgSO4), filtered and concentrated in vacuo.

後処理

  1. washThe mixture was washed with 1M HCl, aq. NaHCO3 and aq. NaCl
  2. dry with materialThe organic layer was dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-fdd2daeea4e04186afc19c09f929978c
出典データセット
uspto-grants-2011_09
特許番号
US08022218B2

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