Fluorosulfuric acid → Difluoromalonyl fluoride

HRID 1447471

反応式

HRID 1447471 の反応式
[F:1][C:2]([F:10])([C:7]([F:9])=[O:8])[C:3](OC)=[O:4].[F:11]S(O)(=O)=O>>[F:10][C:2]([F:1])([C:3]([F:11])=[O:4])[C:7]([F:9])=[O:8]

参加物

3

反応物 2

HCID 24603Fluorosulfuric acidHCID 93396Methyl 2,2,3-trifluoro-3-oxopropanoate

生成物 1

HCID 2774099Difluoromalonyl fluoride収率 66%

実験手順

A mixture of 84 g (0.54 mol) of methyl difluorofluoroformylacetate, 104 g (1.0 mol) of fluorosulfonic acid and 9 g (0.038 mol) of HSbF6 was heated at 100° to 115° for 20 h. Then, 25.6 g of volatile product, collected through a condenser in a -80° trap, and boiling in the range of -25° to +10°, was identified by IR as difluoromalonyl fluoride (66% yield) based on the stoichiometry 2 FOCCF2CO2CH3 :CF2 (COF)2. Dimethyl difluoromalonate was also formed.

後処理

  1. temperaturewas heated at 100° to 115° for 20 h
  2. customThen, 25.6 g of volatile product, collected through a condenser in a -80° trap
  3. customboiling in the range of -25° to +10°

出典と根拠

ORDレコード
ord-df175e990a3e46a0aac702a46a1a72a1
出典データセット
uspto-grants-1982_02
特許番号
US04316986

関連ノート

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