Water → C4F9Och2I

HRID 966862ノート

反応式

HRID 966862 の反応式
[C:1]([O:14][CH2:15]Cl)([C:4]([C:7]([C:10]([F:13])([F:12])[F:11])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2].[I-:17].[Na+].O>CC(C)=O>[C:1]([O:14][CH2:15][I:17])([C:4]([C:7]([C:10]([F:13])([F:12])[F:11])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2]

参加物

5

実験手順

C4F9OCH2Cl (50 g, 0.175 mole, isomer ratio n/i=95:5) was combined with sodium iodide (52.5 g, 0.38 mole) in acetone (200 g) and heated to reflux overnight. Water was added and the acetone distilled from the reaction vessel using a Dean-Stark apparatus. The product was washed with water to remove residual acetone. Glc of the residue (52.6 g) revealed it to be 82.6 wt. % of the desired product C4F9OCH2I, which was further purified by distillation. The distillation fraction boiling at 110-115° C. was found to be 97.8 wt. % of the desired product with a 96/4 normal to iso ratio.

後処理

  1. temperatureheated
  2. temperatureto reflux overnight
  3. distillationthe acetone distilled from the reaction vessel
  4. washThe product was washed with water
  5. customto remove residual acetone
  6. distillationwas further purified by distillation

出典と根拠

ORDレコード
ord-781aa0a380724012ba6dbc1192cfaf35
出典データセット
uspto-grants-2005_10
特許番号
US06953606B2

反応ノート

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