Hydrochloric Acid → 2-Chloro-4-hydroxybenzaldehyde

Temperatur

-78 °C

After 2-chloro-4-hydroxy-benzonitrile (2 g, 0.013 mol) was dissolved in anhydrous THF (40 mL), DIBAL-H 1M hexane solution (21.7 mL, 0.032 mol) was added thereto at −78° C., and the mixture was stirred for 1 hour, and then stirred at room temperature for 2 hours. After the termination of the reaction, the reactant was added with 1M HCl at 0° C. and then extracted with EtOAc. The organic layer was separated, dried with MgSO4, and concentrated under reduced pressure to obtain the title compound, which was used in the next step without a separate purification process.

1. stirringstirred at room temperature for 2 hours
2. customAfter the termination of the reaction
3. extractionextracted with EtOAc
4. customThe organic layer was separated
5. dry with materialdried with MgSO4
6. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-40264fe6f229486c8612a904a343b595

Quelldatensatz

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09447044B2