Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 178502742, 화합물

온도

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 mL), 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 mL), 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 기록

ord-1269af789f834684992516fd2712e1d5

출처 데이터셋

uspto-grants-2000_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06133256