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

HRID 1456320ノート

反応式

HRID 1456320 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 dichlormethane (1 l) and ether (1l). The organics were concentrated in vacuo to give the title compound as a yellow solid (20.7 g).

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 dichlormethane (1 l) and ether (1l)
  6. concentrationThe organics were concentrated in vacuo

出典と根拠

ORDレコード
ord-9bf909261f994b4faf3c1db2e5e27d2f
出典データセット
uspto-grants-1998_12
特許番号
US05843966

反応ノート

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