Hydrochloric Acid → HCID 59699534, Verbindung

The compound (122.6 mg, 0.10 mmol) synthesized in Example 5 (5e) was dissolved in methanol (10 mL) containing 1% aqueous hydrochloric acid solution and 20% palladium hydroxide-carbon (100 mg) was added thereto, followed by stirring of the mixture under a hydrogen atmosphere for 2 hours. After the catalyst was removed by celite filtration, 28% ammonia water (0.5 mL) was added thereto and the mixture was stirred for 10 minutes. After the solvent was distilled off under reduced pressure and the aqueous solution (100 mL) was subjected to ion exchange resin (Dowex 50w×8) column, it was eluted with 1% ammonia water (100 mL). The ammonia water containing the desired compound was concentrated under reduced pressure and the residue was purified using silica gel flash column chromatography (ethyl acetate:methanol:water, 5:2:1-1:1:1, V/V) to obtain the desired title compound (25.9 mg, 56%) as a colorless solid.

1. additionwas added
2. customAfter the catalyst was removed by celite filtration, 28% ammonia water (0.5 mL)
3. additionwas added
4. stirringthe mixture was stirred for 10 minutes
5. distillationAfter the solvent was distilled off under reduced pressure
6. washwas eluted with 1% ammonia water (100 mL)
7. concentrationThe ammonia water containing the desired compound was concentrated under reduced pressure
8. customthe residue was purified

ORD-Eintrag

ord-5d7479b1e3464d93ac7936f2bb218451

Quelldatensatz

uspto-grants-2009_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07632930B2