文档介绍：A1: ADVANCED IDENTIFICATIONS
Attempt to identify pound A and the natural product N.
Warning: Care must be exercised when handling and working with the
'unknown' compounds. As a sensible precaution, assume them to be
hazardous (many are) and avoid any skin contact, inhalation of vapour
or ingestion.
Compound A
i. Purify the material by distillation and/or recrystallisation. Record
the . or, if liquid, the . and the refractive index.
ii. Record the ., . and . spectra.
iii. Submit a sample of your pound for microanalysis. The
submission forms are available at the service counter. Completed forms,
to which a small polytop sample vial containing a few mgs. of your unknown
A is attached, should be handed in via Nick Davies. The form will be
returned to you (after 1-2 weeks) with the correct position
figures and the molecular weight inserted. You will be assessed upon the
accuracy of your results.
iv. Analyse the physical, spectral and microanalytical data in order to
arrive at a structure for the unknown.
v. If at this stage, the identity of pound is still uncertain, it
will be necessary to make a suitable derivative (~100mg). Your data will
have produced alternative structures so choose a derivative which you know
will distinguish between these.
As a safety precaution, discuss the synthesis of the derivative with Dr.
Marsden or Dr. Rzepa before proceding. If necessary, a COSHH assessment
will have to be made.
vi. Propose a structure for A, citing literature data in corroboration.
Compound N
A sample of a natural product (or a simple derivative thereof) is provided
together with its mass spectrum and an accurate mass measurement of the
M+. (Occasionally, no M+ is observed. You will be told if this is the case
and the mass difference from the M+ given).
All the natural products are well-pounds that can be found in
the literature. Remember that the samples provided are not analytical