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Chromatographic separation of some Δ4-3-ketosteroids
✍ Scribed by Tokuichiro Seki
- Publisher
- Elsevier Science
- Year
- 1959
- Tongue
- English
- Weight
- 291 KB
- Volume
- 2
- Category
- Article
- ISSN
- 1873-3778
No coin nor oath required. For personal study only.
✦ Synopsis
Mortite"' is'applied to the lip of the jar 'to provide a seal and to hold in place Im+glass rods 3 mm in: diameter that support the sheets of paper;, Pieces of polyethylene &tubing about z cm long and 3 mm diameter are slit lengthwise-. for use as clips to attach the paper to the rods. Two clips per rod are sufficient support.' If two or three sheets are used per tank no spacers are required; however, if four or five sheets are run simultaneously spacers are needed. The spacers can readily be made of polyethylene (or similar material) by cutting evenly spaced slits 4-5 mm deep into 1.5 mm(I/IG in.)thick strips 10-12 mm wide by 7s mm long. An alternate method of fastening the paper to the rod is by folding the upper edge of the paper over the rod and attaching it by clips made of 1.5 mm (r/16 in.) thick 13 mm square polyethylene. A slit 5-6 mm long is cut into the square. The cut ends of the clip are twisted, parallel to the cut, to ease the insertion of the paper and then twisted in the opposite direction to clamp the paper together.
Solvent is introduced to the bottom of the jar by a long-stemmed funnel, care being taken not to drip any solvent onto the chromatograms. The lid is then pressed into place.
The 12 in. x 12 in. block tanks may be equipped with troughs, supports, etc. for descending chromatography.
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We have developed a new method for the fluorometric determhmtion of A'-fketosteroids. In a methanolic solution of aluminum salt, A'-3-ketosteroids reacted with isonicotinylhydraxine (INH), and the resulting hydrazone fluoresced through complex formation with the aluminum ion in the solution. As lit
DJERASSI, et al. (1) have pointed out that the optical rotatory dispersion (ORD) curve in substituted-A 4 -3-ketosteroids reflects conformational distortions in the B-ring rather than in the A-ring. Their conclusion is based on the observation that 17@-acetoxyandrost-4-en-3-one and its 2,2-dimethyl