Hydrochloric Acid → HCID 57965535, Verbindung

In a 100 ml round-bottomed flask 1-[(1R,3aS,3bS,10aR,10bS,11S,12aS)-7-(4-fluorophenyl)-1,11-dihydroxy-10a,12a-dimethyl-1,2,3,3a,3b,4,5,7,10,10a,10b,11,12,12a-tetradecahydrocyclopenta[5,6]naphtho[1,2-f]indazol-1-yl]-2-hydroxyethanone (Steroids 2003 (68) 177-191) (0.48 g, 1 mmol) was dissolved in MeOH (40 ml). NaOH (6 ml, 1M, 6 mmol) was added and the mixture was stirred vigorously for 6 hours at room temperature in an open vessel. The reaction was monitored by LC-MS. When the reaction was completed the solution was neutralised by the addition of 1M HCl (6 ml, 6 mmol) and the MeOH was removed in vacuo. Water was added to the precipitate (15 ml) and the mixture was stirred for 5 minutes. The solid was then collected by filtration and dried to give 0.4 g (86%) of the desired compound.

1. customthe MeOH was removed in vacuo
2. additionWater was added to the precipitate (15 ml)
3. stirringthe mixture was stirred for 5 minutes
4. filtrationThe solid was then collected by filtration
5. customdried

ORD-Eintrag

ord-d5a023e6caba4f7ebc08f173e91ab92b

Quelldatensatz

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08163724B2