Reaktion #8649

Reaktionsgleichung

acrylonitrile

disodium

naphthalene

sodium

→

Sodium naphthalene

Lösungsmittel

THF

benzene

Tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeis synthesized
2. 2
   Sonstigeanion polymerization
3. 3
   Sonstigeis polymerized
4. 4
   workup.DISTILLATIONare distilled twice using lithium aluminum hydride as a desiccating agent under an argon gas flow
5. 5
   workup.ADDITIONto which molecular sieves 4A is charged
6. 6
   Waschenis washed successively with a saturated aqueous solution of NaHSO3
7. 7
   workup.DISTILLATIONa saturated aqueous solution of NaCl containing 1% of NaOH, and a saturated aqueous solution of NaCl, and then vacuum-distilled
8. 8
   workup.DISTILLATIONfurther vacuum-distilled
9. 9
   workup.ADDITIONto which molecular sieves 4A is charged
10. 10
    TrocknenCrown ether (dicyclohexyl-18-crown-6) is freeze-dried from a solution in benzene
11. 11
    workup.DISSOLUTIONis dissolved in benzene
12. 12
    Trocknenis freeze-dried from a solution in benzene immediately before use

Vorschrift

In this example, a triblock copolymer (PAN-PEO-PAN) consisting of polyethylene oxide (PEO) chain and polyacrylonitrile (PAN) chains is synthesized by living anion polymerization. Using a polyethylene oxide macromer (disodium salt of polyethylene oxide) as a reaction initiator, acrylonitrile is polymerized. Tetrahydrofuran and benzene used as solvents are distilled twice using lithium aluminum hydride as a desiccating agent under an argon gas flow, to which molecular sieves 4A is charged. The acrylonitrile employed as a monomer is washed successively with a saturated aqueous solution of NaHSO3, a saturated aqueous solution of NaCl containing 1% of NaOH, and a saturated aqueous solution of NaCl, and then vacuum-distilled using calcium chloride as a desiccating agent, and further vacuum-distilled using calcium hydride as a desiccating agent under an argon gas flow, to which molecular sieves 4A is charged. Sodium naphthalene is prepared by reacting naphthalene with metallic sodium in THF. Crown ether (dicyclohexyl-18-crown-6) is freeze-dried from a solution in benzene, and then is dissolved in benzene. Polyethylene oxide, which has OH groups at both ends, is freeze-dried from a solution in benzene immediately before use. AS for the polymerization apparatus, a pressure reactor (Taiatsu Glass Co., Ltd.) is employed. The reaction is carefully performed in an argon atmosphere under pressure of 4 atm so as to prevent an external air from entering the interior of the reaction system.

Quelle