Potassium Phosphate, Tribasic → HCID 71543495、化合物

温度

80 °C

To a degassed solution of 2-(4-fluorophenyl)-N-methyl-6-(N-methylmethylsulfonamido)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzofuran-3-carboxamide (110 mg, 0.22 mmol), 2-chloro-12-fluoro-6H-pyrido[2′,3′:5,6][1,3]oxazino[3,4-a]indole (60 mg, 0.220 mmol) and K3PO4 (176 mg, 0.66 mmol) in dioxane/H2O (0.8 mL/0.2 mL) was added Pd2(dba)3 (10 mg, 0.01 mmol) and X-Phos (10 mg, 0.02 mmol) under N2. The mixture was heated to 80° C. and then stirred for 1 hour. The reaction mixture was cooled to RT, diluted with EtOAc and filtered. The filtrate was washed with H2O, brine, dried over Na2SO4. After concentrated, the resulting residue was purified using prep-TLC (petroleum ether:EtOAc=1:1) to provide the desired product of compound 58 (60 mg, yield: 44.4%). 1H-NMR (CDCl3, 400 MHz) δ 7.94˜8.00 (m, 3H), 7.66˜7.68 (m, 2H), 7.46 (s, 2H), 7.29˜7.35 (m, 2H), 7.19 (t, J=8.4 Hz, 3H), 6.02 (s, 1H), 5.91 (s, 2H), 3.39 (s, 3H), 2.98 (d, J=4.8 Hz, 3H), 2.70 (s, 3H). MS (M+H)+: 615.

1. temperatureThe reaction mixture was cooled to RT
2. filtrationfiltered
3. washThe filtrate was washed with H2O, brine
4. dry with materialdried over Na2SO4
5. concentrationAfter concentrated
6. customthe resulting residue was purified

ORDレコード

ord-0e28db1df8df4f69bb34d0015bf542c8

出典データセット

uspto-grants-2016_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09265773B2