CB-Cyclam(M-200) synthesis
- Product Name:CB-Cyclam(M-200)
- CAS Number:130701-19-8
- Molecular formula:C12H26N4
- Molecular Weight:226.36
![1,4,8,11-Tetraazabicyclo[6.6.2]hexadecane, 4,11-bis(phenylmethyl)-](/CAS/20210305/GIF/177937-60-9.gif)
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Yield:130701-19-8 509 mg
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen;acetic acid for 11 h;Sealed tube;
Steps:
28.4 Example 28
(4) Compound (Ab3) (0.90 g), acetic acid (25 mL), and 10% Pd/C (230 mg) were placed in a sealed tube and stirred for 11 hours in a hydrogen atmosphere. Insoluble matter was filtered off, and the solvent was distilled off under reduced pressure. Then, water (30 mL), sodium hydroxide (2 g), and a saturated aqueous solution of sodium chloride (10 mL) were added to the residue, followed by extraction with toluene (50 mL) three times. The solvent was distilled off under reduced pressure to obtain compound (Ab4) (509 mg). LC/MS (ACQUITY) rt (min): 0.20 MS (ESI, m/z): 227.4 [M+H]+ 1H-NMR (300 MHz, CDCl3) δ: 3.73 (1H, brs), 3.11 (2H, ddd, J=2.7, 9.9, 13.2 Hz), 2.59-2.94 (14H, m), 2.34-2.46 (4H, m), 2.26 (1H, brs), 1.85-1.99 (2H, m), 1.25-1.36 (2H, m)
References:
US2016/199520,2016,A1 Location in patent:Paragraph 0436; 0440
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