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CAS No. : | 1334513-02-8 | MDL No. : | MFCD22665799 |
Formula : | C18H17F5NO5P | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 453.30 | Pubchem ID : | - |
Synonyms : |
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Chemical Name : | (S)-Isopropyl 2-(((S)-(perfluorophenoxy)(phenoxy)phosphoryl)amino)propanoate |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338-P310 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
General procedure: To asolution of compound 9a (1.5 g, 4.39 mmol) in tetrahydrofuran(12.0 mL) and 1,3-dimethyltetrahydropyrimidin-2(1H)-one (1.5 mL) at0 C, was added a tetrahydrofuran solution of tert-butylmagnesiumchloride (1 M, 4.39 mL, 4.39 mmol). The resulting suspension wasstirred at 0 C for 30 min and (S)-isopropyl 2-(((S)-(perfluorophenoxy)(phenoxy)phosphoryl)amino)propanoate (3.98 g, 8.78 mmol) wasadded. The resultant mixture was allowed to warm to room temperature.After 1.5 h an aqueous solution of half saturated NaHCO3 (75 mL)and then extracted with ethyl acetate (3×50 mL). The combined organiclayers were dried over MgSO4 and concentrated. The crude productwas purified by flash chromatography on silica eluting with asolvent gradient of 0-5% methanol in dichloromethane to providecompound 16a (2.17 g, 81% yield) containing 6 wt% of 1,3-dimethyltetrahydropyrimidin-2(1H)-one by NMR. 1H NMR (400 MHz,DMSO-d6) delta ppm 1.14 (d, J=6.3 Hz, 6Eta), 1.21 (d, J=7.1 Hz, 3Eta),3.79 (m, 1Eta), 4.00 (m, 1Eta), 4.08 (m, 1Eta), 4.30 (m, 2Eta), 4.84 (m, 1Eta),5.56 (d, J=8.2 Hz, 1Eta), 6.08 (dd, J=13.1, 10.1 Hz, 1Eta), 6.62 (s, 1Eta),6.99 (d, J=5.5 Hz, 1Eta), 7.20 (m, 3Eta), 7.36 (m, 2Eta), 7.63 (d,J=8.1 Hz, 1Eta), 11.58 (s, 1Eta); 13C NMR (101 MHz, DMSO-d6) delta 20.26(d, J=6.5 Hz), 21.84, 21.89, 50.25, 64.58, 68.52, 77.00, 80.23, 84.59,102.55, 120.51 (d, J=4.9 Hz), 125.14, 130.17, 150.72, 151.09 (d,J=6.5 Hz), 163.09, 173.05; 31P NMR (162 MHz, DMSO-d6) delta 3.28. MS(ESI) m/z 612.0 (Mu+Eta)+. |