Formic Acid → HCID 19097008、化合物

HRID 486979

反応式

HRID 486979 の反応式
[F:1][C:2]([F:10])([F:9])[C:3]([C:5]([F:8])([F:7])[F:6])=[CH2:4].[CH:11]1C[CH:14]=[CH:13][CH:12]=1.[OH:16]O.[CH:18]([OH:20])=O>>[OH:16][CH:11]1[CH:18]([OH:20])[CH:14]2[CH2:13][CH:12]1[CH2:4][C:3]2([C:5]([F:8])([F:7])[F:6])[C:2]([F:10])([F:9])[F:1]

参加物

5

反応物 4

HCID 284Formic AcidHCID 784Hydrogen PeroxideHCID 7612CyclopentadieneHCID 914503,3,3-Trifluoro-2-(trifluoromethyl)-1-propene

生成物 1

HCID 19097008HCID 19097008、化合物

反応条件

温度
50 °C

実験手順

5.2 g (20 mmol) of the Diels-Alder reaction product of 3,3,3-trifluoro-2-trifluoromethyl-1-propene (hexafluoroisobutene) and cyclopentadiene are mixed with 20 ml of formic acid, and 1.3 ml of 70 percent strength hydrogen peroxide (30 mmol) is added at 50° C., and the mixture is held at 50° C. for 20 hours. Testing for oxidant using KI-starch paper showed that the oxidant had been broken down completely. The low-boiling components are distilled off under reduced pressure. The residue is heated to 50° C. with 200 ml of 20% strength aqueous sodium hydroxide. The precipitated solid is extracted with a total of 130 ml of methylene chloride. The combined extracts are dried with magnesium sulfate, the methylene chloride is distilled off, and the residue is sublimated at 60° C. in an oil pump vacuum.

後処理

  1. additionis added at 50° C.
  2. distillationThe low-boiling components are distilled off under reduced pressure
  3. extractionThe precipitated solid is extracted with a total of 130 ml of methylene chloride
  4. dry with materialThe combined extracts are dried with magnesium sulfate
  5. distillationthe methylene chloride is distilled off
  6. customis sublimated at 60° C. in an oil pump vacuum

出典と根拠

ORDレコード
ord-af7162bf56cb43e9a873c7fd7f725eb5
出典データセット
uspto-grants-1994_03
特許番号
US05292971

関連ノート

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