HRID1047006

反应详情

EQUATION

反应方程式

HRID 1047006 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl (1-{4-[2-(4-nitrophenyl)-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl]phenyl}cyclobutyl)carbamate (7.70 mg, 0.0128 mmol) was dissolved in DCM (0.5 mL). 4M HCl/dioxane (0.5 mL) was added to the mixture and stirred at room temperature for 4 hours. The mixture was concentrated and solidified with ether. The precipitated solids were collected by filtration and washed with ether to afford desired product (8.04 mg, quant.) as an orange solid. 1HNMR (DMSO-d6) 400 MHz δ: 8.72 (br s, 2H), 8.65 (s, 1H), 8.19-8.14 (m, 2H), 8.13-8.10 (m, 1H), 8.00-7.96 (m, 1H), 7.73-7.68 (m, 2H), 7.62-7.56 (m, 2H), 7.42-7.36 (m, 3H), 7.33-7.29 (m, 1H), 7.18-7.12 (m, 1H), 6.96-6.92 (m, 1H), 6.75 (dd, J=8.0, 4.8 Hz, 1H), 2.69-2.44 (m, 4H), 2.28-2.15 (m, 1H), 1.93-1.78 (m, 1H); LCMS: 501 [M+H].

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. filtrationThe precipitated solids were collected by filtration
  3. washwashed with ether