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 (2 mL) and BOP (2.5 g, 5.6 mmol). The solution was stirred at 0° C. for 10 h. DMF was evaporated in vacuo. 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, washed with cold EtOAc (10 mL) and dried to give Boc—Arg(Tos)—N(Me)OMe (1.5 g, 70% yield). FAB—MS (M+H)+=472

1. customDMF was evaporated in vacuo
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. washwashed with cold EtOAc (10 mL)
10. customdried

ORDレコード

ord-8a687ebb3f5f4b44b0bb57cc1571528d

出典データセット

uspto-grants-2001_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06211154B1