反応 #168743

ord-4eb81eadd4274bd9936c228eb04f5a47

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After completion volatiles were removed under reduced pressure

実験手順

A solution of ((R)-5-{3-bromo-5-[(5-bromo-pyrimidine-2-carbonyl)-amino]-phenyl}-5-methyl-5,6-dihydro-2H-[1,4]oxazin-3-yl)-carbamic acid tert-butyl ester (22 mg, 0.039 mmol) in 4 M HCl in dioxane (0.8 ml, 80 eq.) was warmed to 40° C. for 24 hrs in a closed reaction vial. After completion volatiles were removed under reduced pressure to yield the title compound (hydrochloride salt) in the form of a colourless solid. 1H-NMR (500 MHz, DMSO-d6): 11.05 (s, 1H), 10.61 (s, 1H, NH), 9.25 (s, 2H), 9.19 (s, 1H), 8.58 (s, 1H), 8.26 (s, 1H), 7.89 (s, 1H), 7.44 (s, 1H), 4.59 (m, 2H), 3.91 (m, 2H), 1.63 (s, 3H); MS: 470 [(M+H)+].

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846658B2uspto-grants-2014_09