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 mL), 1 M HCl (10 mL) and sate 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 sate 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-85bf24e075e340e2af219f90ff1c2057

出典データセット

uspto-grants-2001_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06211183B1