Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 178502742、化合物

温度

0 °C

To a suspension of Boc-Arg(Tos)-OH (2 g, 4.7 mmol) in DMF (20 mL) at 0° C. was added MeNHOMe.HCl (1 g, 10.3 mmol), DIEA (6 mL) and BOP (2.5 g, 5.6 mmol). The solution was stirred at 0° C. for 10 hours. DMF was evaporated by vacuum. The oily residue was dissolved in EtOAc (200 mL) and water (20 mL). The organic layer was washed with sat. NaHCO3, water (20 mnL), 1 M HCl ( 10 mL) and sat. NaCl (2×20 mL). The organic layer was dried over MgSO4, filtered and evaporated to give a suspension. The suspension was filtered, and the solid was washed with cold EtOAc (10 mL) and dried to give Boc-Arg(Tos)-N(Me)OMe, shown above, (1.5 g, 70% yield).

1. customDMF was evaporated by vacuum
2. dissolutionThe oily residue was dissolved in EtOAc (200 mL)
3. washThe organic layer was washed with sat. NaHCO3, water (20 mnL), 1 M HCl ( 10 mL) and sat. NaCl (2×20 mL)
4. dry with materialThe organic layer was dried over MgSO4
5. filtrationfiltered
6. customevaporated
7. customto give a suspension
8. filtrationThe suspension was filtered
9. washthe solid was washed with cold EtOAc (10 mL)
10. customdried

ORDレコード

ord-17438e12142449d483b7d1a96736a436

出典データセット

uspto-grants-2001_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06218382B1