Phenylethanolamine → 5-(N-(2-Hydroxy-2-phenylethyl)-2-aminoethyl)amino-2-chloro-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)-benzamide

온도

80 °C

2-Chloro-5-(2-chloroethyl)amino-N-(tricyclo[3.3.1.13,7]dec-1-ylmethyl)benzamide from Example 63 (0.1 g), 2-amino-1-phenylethanol (0.539 g) and triethylamine (0.5 ml) were dissolved in tetrahydrofuran (3 ml) and heated at 80° C. for 60 hours in a sealed tube. The reaction mixture was concentrated under reduced pressure, the residue was suspended in aqueous sodium hydrogen carbonate (30 ml), the product was extracted into ethyl acetate (3×30 ml), dried over magnesium sulphate filtered and concentrated under reduced pressure. Purification by NPHPLC eluting with 0 to 25% ethanol in dichloromethane gave title compound as a white solid (0.044 g).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. extractionthe product was extracted into ethyl acetate (3×30 ml)
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customPurification by NPHPLC
7. washeluting with 0 to 25% ethanol in dichloromethane

ORD 기록

ord-b9cd7a06e44e46adb1dd6f4bc6ee9eda

출처 데이터셋

uspto-grants-2001_03

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06201024B1