Water → C4F9Och2I

HRID 1857898노트

반응식

HRID 1857898 반응식
[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]

참가 물질

5

반응물 3

HCID 962WaterHCID 5238Sodium IodideHCID 9925852Butane, 1-(chloromethoxy)-1,1,2,2,3,3,4,4,4-nonafluoro-

생성물 1

HCID 9951570C4F9Och2I

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0aab472405594b39ab28ef8a173bdefb
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06149980

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