Solanesol phosphamide derivatives and their preparation method and use
A technology for solanesphosphamide and its derivatives, which is applied in the field of solanesphosphamide derivatives and their preparation and application, can solve the problems of poor selectivity and high toxicity, and achieve low toxicity and significant anticancer effects
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Embodiment 1
[0024] Preparation of [(3,4-dimethoxy)benzyl]-N-solanyl-N',N'-bis(2-chloroethyl)diaminophosphate (1) Structure of (1) See Figure 4 , under the protection of nitrogen, add 20mL of dichloromethane and 1.68g (10mmol) of 3,4-dimethoxybenzyl alcohol into the reactor, cool to 0°C, add PCl 3 1.49g (11mmol) and Et 3 N1.01g (10mmol), stirred and reacted for 20 minutes, then added 6.3g (10mmol) of solanesamine, kept the reaction for 60 minutes, then added 1.77g (10mmol) of nitrogen mustard hydrochloride and Et 3 N 1.51 g (15 mmol), continue to keep warm for 60 minutes, then naturally rise to room temperature, and react for 30 minutes. Then cool to -20°C, add 1.9 mL (10 mmol) of 5.2 mol / L decane solution of tert-butanol peroxide, react for 1.5 hours, filter, wash the filter cake with an appropriate amount of water, dry, and purify by silica gel chromatography. Get [(3,4-dimethoxy)benzyl]-N-solanyl-N',N'-bis(2-chloroethyl)diaminophosphate (1); 1 H-NMR (400MHz, DMSO-d 6 ): δ (ppm): 1...
Embodiment 2
[0026] Preparation of [(3,4,5-trimethoxy)benzyl]-N-solanyl-N',N'-bis(2-chloroethyl)diaminophosphate (2):
[0027] (2) structure see Figure 5 , replace the 3,4-dimethoxybenzyl alcohol in Example 1 with 3,4,5-trimethoxybenzyl alcohol, and keep the other things unchanged, prepare [(3,4,5-trimethoxy)benzyl ]-N – solanyl-N', N'-bis(2-chloroethyl) diaminophosphate (2); 1 H-NMR (400MHz, DMSO-d 6 ): δ (ppm): 1.26-1.75 (m, 30H, CH 3 ), 1.96-2.08 (m, 32H, CH 2 ), 2.85-3.38 (m, 7H, NCH 2 , NH), 3.51-3.59 (m, 4H, CH 2 C1), 3.75 (s, 9H, OCH 3 ), 5.10-5.20 (m, 9H, C=CH), 5.28 (s, 2H, CH 2 ), 6.11-6.56 (m, 2H, Ar-H). Anal Calcd for C 59 h 95 Cl 2 N 2 o 5 P : C, 69.87; H, 9.44 N, 2.76. Found: 69.75; H, 9.43; N, 2.76.
Embodiment 3
[0029] Preparation of [[(3-methoxy-4-hydroxy)phenyl]propenyl]-N-solanyl-N',N'-bis(2-chloroethyl)diaminophosphate (3) :
[0030] (3) structure see Image 6 , the 3,4-dimethoxybenzyl alcohol in Example 1 is replaced with 3,4-dimethoxyphenyl propylene alcohol, and other changes are made, and [(3-methoxyl-4-hydroxyl )phenyl]propenyl]-N-solanyl-N',N'-bis(2-chloroethyl)diaminophosphate (3); 1 H-NMR (400MHz, DMSO-d 6 ): δ (ppm): 1.25-1.76 (m, 30H, CH 3 ), 1.96-2.08 (m, 32H, CH 2 ), 2.85-3.38 (m, 7H, NCH 2 , NH), 3.52-3.58 (m, 4H, CH 2 C1), 3.68 (s, 3H, OCH 3 ), 3.74 (s, 3H, OCH 3 ), 5.03-5.20 (m, 9H, C=CH), 5.27 (s, 2H, CH 2 ), 6.58-6.69 (m, 3H, Ar-H). Anal Calcd for C 58 h 93 Cl 2 N 2 o 4 P : C, 70.80; H, 9.46 N, 2.85. Found: 70.73; H, 9.44; N, 2.86.
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