HRID63906

反应详情

EQUATION

反应方程式

HRID 63906 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 5-(1-hydroxy-3-methylbutyl)-1-methyl-3-(3-((tetrahydro-2H-pyran-2-yl)oxy)propyl)-6-(3-(trifluoromethoxy)phenyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (15 mg, 0.026 mmol) in concentrated HCl (1 mL) and MeOH (5 mL) was stirred at RT for 1 h. The reaction was concentrated to a residue which was purified by Prep HPLC to give 5-(1-hydroxy-3-methylbutyl)-3-(3-hydroxypropyl)-1-methyl-6-(3-(trifluoromethoxy)phenyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione (6 mg, 46.9% yield) as a white solid. 1H NMR (CDCl3) δ: 7.49 (t, J=8.0 Hz, 1H), 7.35 (d, J=7.7 Hz, 1H), 7.29 (d, J=8.4 Hz, 1H), 5.39 (d, J=11.9 Hz, 1H), 4.85-4.65 (m, 1H), 4.26 (t, J=6.1 Hz, 2H), 3.70-3.49 (m, 5H), 2.89 (s, 1H), 2.06-1.89 (m, 3H), 1.76 (dt, J=13.4, 6.6 Hz, 1H), 1.43-1.33 (m, 1H), 0.80 (dd, J=9.3 and 6.7 Hz, 6H). LCMS: MH+ 487 and TR=2.971 min.

WORKUP

后处理

  1. concentrationThe reaction was concentrated to a residue which
  2. customwas purified by Prep HPLC