Hydrochloric Acid → 4-(2,4-Difluorophenyl)-2-(2-methylpyrazolo[1,5-a]pyridin-3-yl)-1,3-thiazole-5-carboxylic acid

温度

60 °C

To a suspension of methyl 4-(2,4-difluorophenyl)-2-(2-methylpyrazolo[1,5-a]pyridin-3-yl)-1,3-thiazole-5-carboxylate (250 mg, 0.649 mmol) obtained above in THF (5 mL) and MeOH (5 mL), was added 2N aqueous solution of sodium hydroxide (1 mL) and the mixture was stirred for 2 h at 60° C. To the mixture, was added a 2:1 mixture of EtOAc and THF (60 mL) and 1N hydrochloric acid. The organic layer was separated and the aqueous layer was extracted with a 2:1 mixture of EtOAc and THF (10 mL). The combined organic layers were washed with brine (5 mL) and then dried over anhydrous sodium sulfate. Insoluble materials were removed by filtration and the filtrate was concentrated under reduced pressure to obtain title compound (225 mg, 93%) as a pale yellow solid.

1. additionTo the mixture, was added
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with a 2:1 mixture of EtOAc and THF (10 mL)
4. washThe combined organic layers were washed with brine (5 mL)
5. dry with materialdried over anhydrous sodium sulfate
6. customInsoluble materials were removed by filtration
7. concentrationthe filtrate was concentrated under reduced pressure

ORDレコード

ord-ab43d2760e314fe7973d2d6d47a0038c

出典データセット

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09139589B2