Salicylic Acid → HCID 178454881, Verbindung

HRID 921986

Reaktionsgleichung

Reaktionsgleichung von HRID 921986
[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[OH-].[CH2:12]([P+:16]([CH2:25][CH2:26][CH2:27][CH3:28])([CH2:21][CH2:22][CH2:23][CH3:24])[CH2:17][CH2:18][CH2:19][CH3:20])[CH2:13][CH2:14][CH3:15]>CC(C)=O>[C:1]([O-:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[CH2:25]([P+:16]([CH2:12][CH2:13][CH2:14][CH3:15])([CH2:17][CH2:18][CH2:19][CH3:20])[CH2:21][CH2:22][CH2:23][CH3:24])[CH2:26][CH2:27][CH3:28].[C:1]([OH:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4]

Komponenten

4

Edukt 2

HCID 338Salicylic AcidHCID 84487Phosphonium, tetrabutyl-, hydroxide (1:1)

Produkt 1

HCID 178454881HCID 178454881, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

Salicylic acid (5-20 mmol) and tetrabutylphosphonium hydroxide (˜40% sol. in H2O) (3.414 g, 5 mmol) were dissolved in 20 ml of acetone stirred for 15 min at room temperature. The solvent was evaporated and the remaining viscous liquid was dried under reduced pressure (0.01 mbar, 50° C.) with stirring for 24 hrs. 1H-NMR (300 MHz, d6-DMSO) δ(ppm)=7.74 (dd, J1=7.7 Hz, J2=1.9 Hz, 1H), 7.32 (dt, J1=7.6 Hz, J2=1.8 Hz, 1H), 6.8 (m, 2H), 2.20 (m, 4 H), 1.41 (m, 8 H), 0.9 (t, J=7.1 Hz, 6 H). 31P-NMR (121.5 MHz, d6-DMSO) δ(ppm)=35.1. 13C-NMR (75 MHz, d6-DMSO) δ(ppm)=171.9(s), 163.1(s), 131.1 (d), 129.8(d), 120.6 (s), 115.7 (d), 115.6 (d), 23.3 (d, J=16.4 Hz), 22.6 (d, J=4.8 Hz), 17.3 (d, J=47.3 Hz), 13.2 (s).

Aufarbeitung

  1. customThe solvent was evaporated
  2. customthe remaining viscous liquid was dried under reduced pressure (0.01 mbar, 50° C.)
  3. stirringwith stirring for 24 hrs

Quellen und Nachweise

ORD-Eintrag
ord-79fdd7867a444a6eb52723b3abf9171b
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09278134B2

Verknüpfte Notizen

Wird geladen…