تفاعل #68566

معادلة التفاعل

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

→

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

المذيبات

DCM

TFA

ظروف التفاعل

المعالجة

1. 1
   أخرىSolvents removed under reduced pressure (not-toluene azeotroping
2. 2
   workup.DISSOLUTION) and residue dissolved in CHCl3/IPA (10 mL)
3. 3
   ترشيحSuspension filtered
4. 4
   أخرىProduct purified on silica (12 g)
5. 5
   غسيلeluting with 4-7% of 2M NH3 in MeOH/DCM

الإجراء التجريبي

A solution of tert-butyl 1-(2-chloro-4-(3-((7-methoxyquinolin-4-yloxy)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)ethylcarbamate (100 mg, 178 μmol) in DCM (2 mL) and TFA (2 mL) was stirred for 30 min at 23° C. Solvents removed under reduced pressure (not-toluene azeotroping is suggested!) and residue dissolved in CHCl3/IPA (10 mL). Solution stirred as a suspension with Si-Carbonate (1.3 g; 1 mmol) for 30 min. Suspension filtered and filtrate reduced to an amber film (150 mg). Product purified on silica (12 g) eluting with 4-7% of 2M NH3 in MeOH/DCM. MS (ESI pos. ion) m/z: 461 (MH+). Calc'd exact mass for C24H21ClN6O2: 460.

المصدر