تفاعل #572263

ord-4573794d7611458084fec677ad581975

معادلة التفاعل

CC(=O)O.CCCCO.O
n-butanol acetic acid water
O=C(O)CCCN1CCN[C@@H](C(=O)O)C1
D-CPC
CCO
EtOH
O=C1c2ccccc2C(=O)C1(O)O
ninhydrin

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلThe column is washed with 80 l of water
  2. 2
    أخرىThe eluate is collected in 8 l fractions which
  3. 3
    أخرىThe HPLC gives an elution curve corresponding to the first half of the attached drawing
  4. 4
    غسيلare eluted in two distinct patterns
  5. 5
    غسيلto elute CPC
  6. 6
    أخرىobtain a better-defined elution curve
  7. 7
    أخرىthe eluate is collected in 8 l fractions
  8. 8
    أخرىthere is obtained an elution curve corresponding to the second half of the drawing
  9. 9
    أخرىdried in air

الإجراء التجريبي

The column is washed with 80 l of water, followed by passage of 240 l of 0-10% EtOH at SV=1.0 (80 l/hr.). The eluate is collected in 8 l fractions which are assayed by HPLC. The HPLC gives an elution curve corresponding to the first half of the attached drawing. It is clear that D-CPC and DA-CPC are eluted in two distinct patterns. A further amount of 10% EtOH may be passed to elute CPC but in order to save on the elution time and obtain a better-defined elution curve, the eluant is replaced with 20% EtOH and the eluate is collected in 8 l fractions. As assayed by HPLC, there is obtained an elution curve corresponding to the second half of the drawing. Each fraction is applied to a thin-layer chromatoplate of microcrystalline cellulose powder (Tokyo Kasei K.K. Japan) and the chromatogram is developed with n-butanol-acetic acid-water (3:1:1, V/V), and dried in air. The image formed by color-reaction with ninhydrin shows a spot each at Rf=0.15 for D-CPC, RF=0.28 for CPC and Rf=0.30 for DA-CPC.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04535155uspto-grants-1985_08