Diisopropylethylamine → 3-(4-(3-(4-chloro-2-fluorophenoxy)azetidin-1-yl)-1,3,5-triazin-2-ylamino)-N-methylbenzamide

温度

80 °C

To a solution of 2-chloro-4-(3-(4-chloro-2-fluorophenoxy)azetidin-1-yl)-1,3,5-triazine (0.800 g, 2.54 mmol) in Isopropanol (8 mL) was added DIPEA (0.7 mL, 3.81 mmol) and 3-amino-N-methylbenzamide (0.382 g, 2.54 mmol) and the reaction mixture was stirred at 80° C. for 24 h. The mixture was concentrated under reduced pressure and extracted with EtOAc (2×40 mL). The organic extracts were washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. Purification by silica gel column chromatography to obtain 3-(4-(3-(4-chloro-2-fluorophenoxy)azetidin-1-yl)-1,3,5-triazin-2-ylamino)-N-methylbenzamide (0.527 g, 53%) as a solid. Observed mass (M+1): 428.9

1. concentrationThe mixture was concentrated under reduced pressure
2. extractionextracted with EtOAc (2×40 mL)
3. washThe organic extracts were washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customPurification by silica gel column chromatography

ORDレコード

ord-853735f6ddee47d6a849f5e942536827

出典データセット

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09334269B2