反応 #60361

反応方程式

6-Piperidin-1-ylmethyl-1,2,3,4-tetrahydro-naphthalen-2-ylamine bis-TFA salt

3-(naphthalen-2-yl-sulfonylamino)-3-phenyl-propionic acid

HOBt

EDC

→

title compound

3-(naphthalen-2-yl-sulfonylamino)-3-phenyl-N-(6-piperidin-1-ylmethyl-1,2,3,4-tetrahydro-naphthalen-2-yl)-propionamide

溶媒

CH2Cl2

反応条件

後処理

1. 1
   workup.STIRRINGthe reaction was stirred at RT until HPLC analysis
2. 2
   その他consumption of starting material
3. 3
   workup.ADDITIONThe reaction mixture was diluted with CH2Cl2
4. 4
   洗浄washed with saturated aqueous NaHCO3
5. 5
   乾燥The organic layer was dried over MgSO4
6. 6
   濃縮concentrated in vacuo
7. 7
   その他to afford the crude material
8. 8
   その他The crude was purified by flash column chromatography

実験手順

6-Piperidin-1-ylmethyl-1,2,3,4-tetrahydro-naphthalen-2-ylamine bis-TFA salt (Step F) (0.143 g, 0.327 mmol), 3-(naphthalen-2-yl-sulfonylamino)-3-phenyl-propionic acid (0.128 g, 0.360 mmol), HOBt (0.057 g, 0.425 mmol) and EDC (0.081 g, 0.425 mmol) were dissolved in CH2Cl2 (25 mL) and stirred at RT. TEA (0.228 mL, 1.64 mmol) was added drop-wise to the mixture and the reaction was stirred at RT until HPLC analysis showed complete consumption of starting material. The reaction mixture was diluted with CH2Cl2 and washed with saturated aqueous NaHCO3. The organic layer was dried over MgSO4 and concentrated in vacuo to afford the crude material. The crude was purified by flash column chromatography to furnish the title compound. MS (APCI pos) 582 (M+H).

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