Potassium Carbonate → HCID 86705363, Verbindung

Temperatur

70 °C

To a stirred solution of 2.01 g (5 mmol) 6,8-dibromo-3-iodoimidazo[1,2-b]pyridazine which was prepared according to intermediate example 96c in NMP (15 mL) were added 1.94 g (15 mmol) DIPEA and 1.30 g (10 mmol) 2-(morpholin-4-yl)ethanamine in one portion at rt. After heating for 2 h at 70° C., 100 mL DCM were added and the mixture was washed with water (3×100 mL). The organic phase was dried over sodium sulphate and evaporated to yield a brownish solid which was used without further purification in the next step. To a stirred solution of the remaining solid in 20 mL THF were added 1.16 g (6 mmol) [3-methyl-4-(methylcarbamoyl)phenyl]boronic acid which was prepared according to intermediate example 562b, 15 mL aqueous potassium carbonate solution (15 mmol, 1M), 816 mg Pd(dppf)Cl2 (1 mmol) and the mixture was heated for 41 h at 70° C., to yield after working up and purification 2.35 g (99%) of the title compound.

1. washthe mixture was washed with water (3×100 mL)
2. dry with materialThe organic phase was dried over sodium sulphate
3. customevaporated
4. customto yield a brownish solid which
5. customwas used without further purification in the next step
6. customwas prepared
7. temperaturethe mixture was heated for 41 h at 70° C.
8. customto yield
9. custompurification 2.35 g (99%) of the title compound

ORD-Eintrag

ord-e43fa7be1a60476cb17dc9d3c50c88fe

Quelldatensatz

uspto-grants-2016_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09255100B2