Triethylamine → HCID 22628483, Verbindung

Temperatur

100 °C

To a stirred solution of Pd (OAc)2 (40 mg, 0.18 mmol), nBu3P (71 mg, 0.35 mmol), and Et3N (232 mg, 2.29 mmol) in DMF (5 ml) was added 3-butene-1,2-diol (155 mg, 1.76 mmol) followed by 4-iodotoluene (500 mg, 2.29 mmol), and the reaction mixture was stirred at 100° C. for 1.5 h. The reaction mixture was poured into water (50 ml) and extracted with ethyl acetate. The organic layer was washed with brine, dried (magnesium sulfate) and evaporated in vacuo. The residue was purified by silica gel (10 g) column chromatography eluting with toluene/ethyl acetate (50:1) to give 1-hydroxy-4-(p-tolyl)butan-2-one (230 mg, 73.4%) as a pale yellow solid.

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried (magnesium sulfate)
4. customevaporated in vacuo
5. customThe residue was purified by silica gel (10 g) column chromatography
6. washeluting with toluene/ethyl acetate (50:1)

ORD-Eintrag

ord-5ddef9eff4e543c39820720f77525efe

Quelldatensatz

uspto-grants-2002_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06359145B1