S News Some tips on 630-17-1

According to the analysis of related databases, 630-17-1, the application of this compound in the production field has become more and more popular.

Related Products of 630-17-1, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 630-17-1 as follows.

Example 21; 2-tert-Butyl-l-[(4,4-difluorocycIohexyl)methyl]-5-{[4-(2,2-dimethyIpropoxy)piperidin- l-yl]carbonyl}-lH-benzimidazole; To a solution of NaH (0.017 g, 0.414 mmol) in 2 mL of DMF at 0C under nitrogen, a DMF solution (2 mL) of l-({2-ter/-butyl-l-[(4,4-difluorocyclohexyl)methyl]-lH-benzimidazol-5- yl}carbonyl)piperidin-4-ol (for preparation, see Example 16, Step B) (0.060 g, 0.138 mmol) was added dropwise. The solution was stirred at O0C under nitrogen for 30 min. 1-Bromo- 2,2-dimethylpropane (0.035 mL, 0.276 mmol) was added dropwise and the solution was stirred at 1000C overnight. The reaction was quenched at 00C by addition of aqueous saturated NaHCOs solution and the solvent was concentrated. The residue was dissolved in EtOAc and washed with saturated aqueous NaHCC>3 solution, brine and dried over anhydrous Na2SO4. The product was purified by reversed-phase HPLC using 20-50% CH3CN/H2O and lyophilized to afford the title compound as the corresponding TFA salt. Yield: 45 mg (53%); 1H NMR (400 MHz, METHANOL-D4) delta 0.89 – 0.93 (m, 9 H), 1.51 – 1.64 (m, 2 H), 1.65 – 1.70 (m, 10 H), 1.70 – 1.85 (m, 6 H), 1.94 (s, 1 H), 2.01 – 2.12 (m, 2 H), 2.20 – 2.32 (m, 1 H), 3.14 (d, /=8.59 Hz, 2 H), 3.32 (s, 1 H), 3.54 – 3.62 (m, 2 H), 3.67 (s, 1 H), 3.93 (s, 1 H), 4.57 (d, /=7.62 Hz, 2 H), 7.62 (dd, /=8.69, 1.46 Hz, 1 H), 7.78 (d, /=0.98 Hz, 1 H), 7.99 (d, /=8.59 Hz, 1 H); MS (ESI) (M+H)+ 504.3.

According to the analysis of related databases, 630-17-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ASTRAZENECA AB; WO2007/145563; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary