3-Amino-1-propanol → HCID 66773976, Verbindung

Temperatur

45 °C

To a solution of bromo-(4-fluoro-phenyl)-acetic acid methyl ester (16.0 g) in chloroform (100 mL) was added potassium carbonate (17.9 g, finely ground) followed by 3-amino-1-propanol (4.87 g). The reaction was heated to 45° C. for 18 hours. The reaction was filtered and the filtrate was diluted with water and the phases were separated. The aqueous phase was further extracted with chloroform (3×25 mL) and the combined organics were washed with brine. The chloroform phase was dried over sodium sulfate, filtered and evaporated in vacuo to give the desired (4-fluoro-phenyl)-(3-hydroxy-propylamino)-acetic acid methyl ester (14.85 g, MS (ES+): 242.2 (MH+)) as a yellow oil which was used in the next step without further purification.

1. filtrationThe reaction was filtered
2. additionthe filtrate was diluted with water
3. customthe phases were separated
4. extractionThe aqueous phase was further extracted with chloroform (3×25 mL)
5. washthe combined organics were washed with brine
6. dry with materialThe chloroform phase was dried over sodium sulfate
7. filtrationfiltered
8. customevaporated in vacuo

ORD-Eintrag

ord-40afdde3d9d34abb9f55f3d86697f01a

Quelldatensatz

uspto-grants-2012_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08124636B2