Hydrochloric Acid → 4-[N-Cyclopropylmethyl-(6a-methyl-5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)amino]benzoic acid

Temperatur

50 °C

A suspension of ethyl 4-[N-cyclopropylmethyl-(6a-methyl-5,6,6a,7,8,9-hexahydro-4H-2-phenalenyl)amino]benzoate (0.063 g) in ethanol (5 ml) was added with 20% aqueous sodium hydroxide (1 ml), and the mixture was stirred overnight at 50° C. The reaction mixture was left to cool and then made acidic with 2 N aqueous hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was recrystallized from chloroform-n-hexane to obtain the title compound (0.042 g, yield: 71%) as colorless needles (melting point: 234-235° C.).

1. waitThe reaction mixture was left
2. temperatureto cool
3. extractionthe mixture was extracted with chloroform
4. washThe organic layer was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationThe organic layer was concentrated under reduced pressure
7. customthe resulting residue was recrystallized from chloroform-n-hexane

ORD-Eintrag

ord-7727f0ece7d54f3b974035f06d97d108

Quelldatensatz

uspto-grants-2012_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08143260B2