Reaktionsgleichung
C(O)(O)CCCCC.C(Br)CCCCCCC.C(OCCCCCCOC(C)=O)CCCCCCC.[C:37]([O:62][C:63]([C:66]([C:69]([C:72]([C:75](C(O)=O)([F:77])[F:76])([F:74])[F:73])([F:71])[F:70])([F:68])[F:67])([F:65])[F:64])([C:40]([C:43]([C:46]([C:49]([C:52]([C:55]([C:58]([F:61])([F:60])[F:59])([F:57])[F:56])([F:54])[F:53])([F:51])[F:50])([F:48])[F:47])([F:45])[F:44])([F:42])[F:41])([F:39])[F:38]>>[C:37]([O:62][C:63]([C:66]([C:69]([C:72]([CH:75]([F:76])[F:77])([F:73])[F:74])([F:70])[F:71])([F:67])[F:68])([F:65])[F:64])([C:40]([C:43]([C:46]([C:49]([C:52]([C:55]([C:58]([F:61])([F:60])[F:59])([F:57])[F:56])([F:54])[F:53])([F:51])[F:50])([F:48])[F:47])([F:45])[F:44])([F:42])[F:41])([F:39])[F:38]Komponenten
5
Reaktionsbedingungen
- Temperatur
- 185 °C
Versuchsvorschrift
In a fashion similar to Example 8, hexanediol was alkylated with n-octyl bromide, the product was acetylated, and the resulting C8H17—O—(CH2)6—O—COCH3 was directly fluorinated and hydrolyzed as in Example 8 to C8F17—O—(CF2)5COOH, which was recrystallized from perfluorohexane. The recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol and heated to 185° C. The product was washed with water, and the residual 27.9 g was distilled to give pure C8F17—O—(CF2)5H, micro b.p. 195° C.
Aufarbeitung
- customwas recrystallized from perfluorohexane
- additionThe recrystallized acid (37.5 g) was mixed with 4.0 g NaOH and 100 mL ethylene glycol
- washThe product was washed with water
- distillationthe residual 27.9 g was distilled
Quellen und Nachweise
- ORD-Eintrag
- ord-da5e77db1c384d33b081993809ef24ee
- Quelldatensatz
- uspto-grants-2002_03
- Patentnummer
- US06361713B1
Verknüpfte Notizen
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