n-PROPYL NITRATE → 2,4-Dibenzyloxybenzonitrile

HRID 322860

Reaktionsgleichung

Reaktionsgleichung von HRID 322860
[CH2:1]([O:8][C:9]1[CH:16]=[C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:14]=[CH:13][C:10]=1[CH:11]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P([O-])([O-])(O)=O.[NH4+].[NH4+].[N+:32]([O-])(OCCC)=O>C(O)(=O)C>[CH2:1]([O:8][C:9]1[CH:16]=[C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:14]=[CH:13][C:10]=1[C:11]#[N:32])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 12307n-PROPYL NITRATEHCID 24540Diammonium hydrogen phosphateHCID 18090802,4-Bis(benzyloxy)benzaldehyde

Produkt 1

HCID 103136042,4-DibenzyloxybenzonitrileAusbeute 40 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A mixture of 2,4-dibenzyloxybenzaldehyde (1.59 g), diammonium hydrogen phosphate (3.5 g) and n-propyl nitrate (15 mL) in glacial acetic acid (5 mL) is refluxed for 15 hours. The reaction mixture is evaporated to dryness in vacuo and the residue is stirred with water (100 mL). The insoluble material is filtered and dried at 50° C. to yield 2,4-dibenzyloxybenzonitrile as a tan coloured solid (0.6 g, 40%), m.p. 100° C. [Elemental analysis:- C,79.8; H,5.47; N,4.48%. Calculated:- C,80.0; H,5.43; N,4.44%].

Aufarbeitung

  1. temperatureis refluxed for 15 hours
  2. customThe reaction mixture is evaporated to dryness in vacuo
  3. filtrationThe insoluble material is filtered
  4. customdried at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-9831dfc070f94d43ac3683f15f5f4b2f
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06211234B1

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