1,2-Dichloroethane → 4-Chlorobenzhydrol

To a solution of 1-[(4-chloro-phenyl)-phenyl-methyl]-piperazine (0.59 g, 2.08 mmol) in dry CH2Cl2 (40 ml) was added 3,3-diphenylpropanoic acid (0.472 g, 2.08 mmol) under nitrogen. To the reaction was added EDC (0.797 g, 4.16 mmol) and DMAP (cat) and the reaction mixture stirred under nitrogen at room temp. over night. The reaction was then concentrated under reduced pressure. The residue dissolved in ethyl acetate: water (10:1) (150 ml). The organic was washed with water (30 ml, 2×) and 10% NaOH (30 ml) and dried over MgSO4 and evaporated to dryness. The resulting residue was purified by column chromatography using hexane: ethyl acetate (3:1) to give desired product in 78% yield.

1. concentrationThe reaction was then concentrated under reduced pressure
2. dissolutionThe residue dissolved in ethyl acetate: water (10:1) (150 ml)
3. washThe organic was washed with water (30 ml, 2×) and 10% NaOH (30 ml)
4. dry with materialdried over MgSO4
5. customevaporated to dryness
6. customThe resulting residue was purified by column chromatography

ORD-Eintrag

ord-8880e1cd7dbf471a8968b80625732fc8

Quelldatensatz

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06949554B2