2-Hydroxy-Δ^1,4-3-keto Steroids

Remangilone D, a New Bisnoroleanane Triterpene, and a New Flavone from Physena madagascariensis [1]

“…O th er long-range h etero n u clear couplings (l"-H /C -8 , C-7, C -8 a, and 2"-H/C-8) w ere in accord with this structure. 99.3 (d) 6.32 (s) C-4a, C-5, C-7, C- 8 7 162.8 (s) C-2", C-3", C-5", C-6 ' 1 ', C-7" 5"…”

“…Flavone 6 was isolated from the previously described [1,4] chrom atographic frac tion "F 8 " of th e 30% aqueous m eth an o l soluble fraction (9 g) o f th e crude m ethanol extract. Flash chrom atog rap h y of F 8 (720 mg) on silica gel using a step grad ien t of aceto n e in hexanes (5% ace tone -2 0 0 ml, 1 0 % aceto n e -2 0 0 ml, 2 0 % ace tone -200 ml, and 40% acetone -100 ml) gave four fractions ("F8-1" through "F8-4") with "F8-2", eluting w ith 20% acetone, containing 6 . Flash ch ro m ato g rap h y o f "F8-2" on C 1 8 reversed phase silica gel eluting w ith a step gradient of m ethanol (50% -100 ml, 60% -100 ml, 70% -130 ml, 80% -100 m l and 100% m ethanol -…”

“…EIMS fragmentation of6 .Experimental SectionGeneral experim ental proceduresThe X H and 13C N M R spectra w ere recorded at 93.94 k G (*H 400 M H z, 13C 100 M H z) and 70.5 kG (13C 75 M H z) at am bient tem perature. Chem ical shifts are expressed in ppm relative to internal re f erence: for *H N M R spectra, the residual CHC13 resonance at <3 = 7.24 or residual C H D2 C O C D 3 resonance at d = 2.05, for 13C N M R, the center line of th e solvent triplet at (5 = 77.0 for CDC13, and the cen ter line of the solvent septet at d = 29.9 for acetone-d6.…”

Selenium dioxide oxidation of olefins

“…Solvolysis of this ester (4,5) would produce the product observed and result in equilibration of the benzylic positions.…”

Reaktionen mit Blei(IV)‐acetat, XVI. Eine neuartige Umwandlung von 2‐Acetoxy‐3‐oxo‐4,5‐epoxy‐steroiden

“…IJV.-Spektrum: Amax 254 nm ( E = 15500) (Lit. : 254/15400 [18]; 254/15140 [19]; 259, 290/14600, 3100 [20]). 1R.-Spektrum: Banden u.a.…”