Formic Acid → 2,3-Dihydroxy-5-(perfluorohexyl)bicyclo[2.2.1]heptane

HRID 486981ノート

反応式

HRID 486981 の反応式
[F:1][C:2]([F:21])([C:5]([F:20])([F:19])[C:6]([F:18])([F:17])[C:7]([F:16])([F:15])[C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10])[CH:3]=[CH2:4].[CH:22]1C[CH:25]=[CH:24][CH:23]=1.[OH:27]O.[CH:29]([OH:31])=O>>[OH:27][CH:22]1[CH:29]([OH:31])[CH:25]2[CH2:24][CH:23]1[CH2:4][CH:3]2[C:2]([F:21])([F:1])[C:5]([F:19])([F:20])[C:6]([F:17])([F:18])[C:7]([F:15])([F:16])[C:8]([F:13])([F:14])[C:9]([F:12])([F:11])[F:10]

参加物

5

反応物 4

HCID 284Formic AcidHCID 784Hydrogen PeroxideHCID 7612CyclopentadieneHCID 91384(Perfluorohexyl)ethylene

生成物 1

HCID 190970052,3-Dihydroxy-5-(perfluorohexyl)bicyclo[2.2.1]heptane

実験手順

8.2 g (20 mmol) of the Diels-Alder reaction product of 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluoro-1-octene (perfluorohexylethene) and cyclopentadiene are mixed with 20 ml of formic acid, 1.3 ml of 70 percent strength hydrogen peroxide (30 mmol) is added at 60° C., and the mixture is held at 60° C. for 36 hours. The low-boiling components are distilled off in vacuo. The residue is extracted with three portions (130 ml in total) of methylene chloride. The combined extracts are dried with magnesium sulfate and the methylene chloride is removed in vacuo. The residue is sublimed at 95° C. in an oil pump vacuum.

後処理

  1. additionis added at 60° C.
  2. distillationThe low-boiling components are distilled off in vacuo
  3. extractionThe residue is extracted with three portions (130 ml in total) of methylene chloride
  4. dry with materialThe combined extracts are dried with magnesium sulfate
  5. customthe methylene chloride is removed in vacuo
  6. customis sublimed at 95° C. in an oil pump vacuum

出典と根拠

ORDレコード
ord-d181e0f70cb34459820915525b70489f
出典データセット
uspto-grants-1994_03
特許番号
US05292971

反応ノート

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