تفاعل #68563

معادلة التفاعل

(R)—N—((S)-1-(2-chloro-4-(3-((7-methoxyquinolin-4-yloxy)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)-2,2,2-trifluoroethyl)-2-methylpropane-2-sulfinamide

→

(S)-1-(2-chloro-4-(3-((7-methoxyquinolin-4-yloxy)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)-2,2,2-trifluoroethanamine

المذيبات

MeOH

HCl

ظروف التفاعل

المعالجة

1. 1
   أخرىSolvents removed under reduced pressure
2. 2
   أخرىwith azeotroping from toluene
3. 3
   workup.DISSOLUTIONResidue dissolved in MeOH (10 mL)
4. 4
   ترشيحfiltrated
5. 5
   ترشيحcollected by filtration
6. 6
   أخرىSolvents removed under reduced pressure and residue
7. 7
   أخرىpurified on silica (12 g)
8. 8
   غسيلeluting product with 0>5% MeOH/DCM

الإجراء التجريبي

A solution of (R)—N—((S)-1-(2-chloro-4-(3-((7-methoxyquinolin-4-yloxy)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)-2,2,2-trifluoroethyl)-2-methylpropane-2-sulfinamide (135 mg, 218 μmol) in MeOH (2 mL) and 4M HCl (2 mL) was stirred for 30 min at 35° C. LCMS suggests full conversion. Solvents removed under reduced pressure with azeotroping from toluene. Residue dissolved in MeOH (10 mL) and Si-Carbonate (2 g; 1.4 mmol) added. Suspension stirred for 30 min, then filtrated collected by filtration. Solvents removed under reduced pressure and residue purified on silica (12 g) eluting product with 0>5% MeOH/DCM. MS (ESI pos. ion) m/z: 515 (MH+). Calc'd exact mass for C24H18ClF3N6O2: 514.

المصدر