Acetonitrile → Phthalonitrile

HRID 240206

Reaktionsgleichung

Reaktionsgleichung von HRID 240206
[NH2:1][C:2]1[C:3](S(O)(=O)=O)=[CH:4][CH:5]=[C:6](S(O)(=O)=O)[CH:7]=1.[C:16](#[N:18])[CH3:17]>O>[C:2](#[N:1])[C:7]1[C:17](=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:16]#[N:18]

Komponenten

4

Edukt 2

HCID 6342AcetonitrileHCID 609882-Amino-p-benzenedisulfonic acid

Produkt 1

HCID 7042Phthalonitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

A solution of aniline 2,5 disulphonic acid (27.5 g) in water (250 ml) was added to intermediate E (63.2 g) in acetonitrile (800 ml) and heated at 40° C. and at pH 5 to 7 overnight. The reaction solvent was removed under reduced pressure, water (50 ml) was added and then brine (60 ml) the solid which precipitated of filtered off, washed with 10% brine and dried to give product (91.1% strength, 22 g).

Aufarbeitung

  1. customThe reaction solvent was removed under reduced pressure, water (50 ml)
  2. additionwas added
  3. custombrine (60 ml) the solid which precipitated
  4. filtrationof filtered off
  5. washwashed with 10% brine
  6. customdried
  7. customto give product (91.1% strength, 22 g)

Quellen und Nachweise

ORD-Eintrag
ord-fe1ef58b8c64429ab6caf2f77af6a2c5
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08647425B2

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