Carbamate → HCID 22669293, Verbindung

The crude carbamate (0.257 g, 0.84 mmol) was deprotected by stirring in 4N HCl—dioxane (15 mL) for 2 h at room temperature. Volatiles were removed under reduced pressure to give a pinkish solid. 4-Formylphenoxyacetic acid (0.200 g, 1.1 mmol) was dissolved in DCM (3 mL) and DIEA (0.5 mL) was added followed by TBTU (0.350 g, 1,1 mmol) and the amine salt from above (0.240 g, 1 mmol). The mixture was stirred 4 h at room temperature, dissolved in EtOAc and washed sequentially with 5% aqueous K2CO3, KHSO4, water and brine. The extract was dried (MgSO4) and concentrated under reduced pressure to give an off-white solid (0.162 g).

1. customVolatiles were removed under reduced pressure
2. customto give a pinkish solid
3. washwashed sequentially with 5% aqueous K2CO3, KHSO4, water and brine
4. dry with materialThe extract was dried (MgSO4)
5. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-0c14e45ea2ed416b9b0bdded8b4b7d95

Quelldatensatz

uspto-grants-2008_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07439258B2