반응 #971539

반응 방정식

(S)-tert-butyl 3-((S)-6-(2-hydroxy-2-methylpropyl)-2-oxo-6-phenyl-1,3-oxazinan-3-yl)piperidine-1-carboxylate

→

(S)-6-(2-hydroxy-2-methylpropyl)-6-phenyl-3-((S)-piperidin-3-yl)-1,3-oxazinan-2-one

용매

TFA CH2Cl2

반응 조건

후처리

1. 1
   농축The mixture was concentrated
2. 2
   workup.DISSOLUTIONredissolved in CH2Cl2 (25 mL)
3. 3
   세척washed with satd aq NaHCO3 solution (10 mL), brine (8 mL)
4. 4
   건조dried over Na2SO4
5. 5
   여과After filtration and concentration
6. 6
   기타the crude (S)-6-(2-hydroxy-2-methylpropyl)-6-phenyl-3-((S)-piperidin-3-yl)-1,3-oxazinan-2-one as its TFA salt which was used without further purification

실험 절차

(S)-tert-butyl 3-((S)-6-(2-hydroxy-2-methylpropyl)-2-oxo-6-phenyl-1,3-oxazinan-3-yl)piperidine-1-carboxylate (25 mg, 0.058 mmol) was dissolved in 20% TFA/CH2Cl2 (8 mL) solution and stirred 30 min at rt. The mixture was concentrated, redissolved in CH2Cl2 (25 mL), washed with satd aq NaHCO3 solution (10 mL), brine (8 mL), dried over Na2SO4. After filtration and concentration, the crude (S)-6-(2-hydroxy-2-methylpropyl)-6-phenyl-3-((S)-piperidin-3-yl)-1,3-oxazinan-2-one as its TFA salt which was used without further purification. LC-MS Method 1 tR=0.86 min., m/z 333 (M+1).

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