Lithium Hydroxide → 6-Tert-butyl-8-fluoro-2-[3-(hydroxymethyl)-4-[1-methyl-5-[(5-methyloxazol-2-yl)amino]-6-oxo-3-pyridyl]-2-pyridyl]phthalazin-1-one

温度

35 °C

A mixture of 125b (114 mg, 0.20 mmol) and lithium hydroxide (120 mg, 5.0 mmol) in i-propanol/THF/water (2:2:1, 10 mL) was stirred at 35° C. for 30 mins. The mixture was concentrated under reduced pressure and the residue was diluted with water (5 mL). The resulting mixture was extracted with dichloromethane three times. The combined organic layer was then concentrated under reduced pressure and the resulting residue was purified by reverse-phase prep-HPLC to afford 125 (52 mg, 49%). MS-ESI: [M+H]+ 530.9. 1H NMR (500 MHz, DMSO-d6) δ 9.25 (s, 1H), 8.57 (d, J=5.0 Hz, 1H), 8.53 (d, J=3.0 Hz, 1H), 8.25 (d, J=2.5 Hz, 1H), 7.90 (d, J=1.0 Hz, 1H), 7.78 (dd, J=1.0, 13.0 Hz, 1H), 7.61 (d, J=2.0 Hz, 1H), 7.50 (d, J=5.0 Hz, 1H), 6.64 (d, J=1.5 Hz, 1H), 4.92 (bs, 1H), 4.40 (d, J=7.0 Hz, 2H), 3.60 (s, 3H), 2.22 (s, 3H), 1.39 (s, 9H).

1. concentrationThe mixture was concentrated under reduced pressure
2. additionthe residue was diluted with water (5 mL)
3. extractionThe resulting mixture was extracted with dichloromethane three times
4. concentrationThe combined organic layer was then concentrated under reduced pressure
5. customthe resulting residue was purified by reverse-phase prep-HPLC

ORDレコード

ord-867d472c8a60430480a991b936f993ec

出典データセット

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08669251B2