Carbon Tetrachloride → N-(4-Benzyloxy-phenyl)-2,2,2-trifluoro-acetimidoyl chloride

HRID 1941506ノート

反応式

HRID 1941506 の反応式
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:20]([O:27][C:28]1[CH:33]=[CH:32][C:31]([NH:34][C:35](=O)[C:36]([F:39])([F:38])[F:37])=[CH:30][CH:29]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.C(Cl)(Cl)(Cl)[Cl:42]>>[CH2:20]([O:27][C:28]1[CH:33]=[CH:32][C:31]([N:34]=[C:35]([Cl:42])[C:36]([F:39])([F:38])[F:37])=[CH:30][CH:29]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

4

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 21197250N-(4-Benzyloxy-phenyl)-2,2,2-trifluoro-acetamide

生成物 1

HCID 21197258N-(4-Benzyloxy-phenyl)-2,2,2-trifluoro-acetimidoyl chloride

実験手順

A mixture of resin-supported triphenylphosphine (3 mmol triphenylphosphine/g resin; 58.6 g) and N-(4-benzyloxy-phenyl)-2,2,2-trifluoro-acetamide in carbon tetrachloride (800 ml) was heated to reflux under nitrogen for 18 h. The mixture was allowed to cool then filtered, washing the resin with dichloromethane (1l) and ether (1l). The organics were concentrated in vacuo to give the title compound as a yellow solid (20.7 g). T.l.c. (Cyclohexanelethyl acetate (9:1)) Rf 0.81

後処理

  1. temperaturewas heated
  2. temperatureto reflux under nitrogen for 18 h
  3. temperatureto cool
  4. filtrationthen filtered
  5. washwashing the resin with dichloromethane (1l) and ether (1l)
  6. concentrationThe organics were concentrated in vacuo

出典と根拠

ORDレコード
ord-5f6274e27f8f4682834b29df24f95f0c
出典データセット
uspto-grants-1997_12
特許番号
US05703240

反応ノート

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