Lithium Hydroxide → HCID 89720667、化合物

To a 200 mL flask containing (S)-2-[4-[[3,5-difluoro-4-[(S)-1-propoxycarbonyl-2-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]ethylcarbamoyl]benzylamino]methyl]-2,6-difluorobenzoylamino]-3-[4-[1,3,6-trimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidin-5-yl]phenyl]propionic acid propyl ester (1004 mmg, 0.97 mmol) was added THF (25 mL), water (25 mL) and LiOH (193 mg, 4.6 mmol) and the reaction stirred at room temperature overnight. The reaction was concentrated, dried from acetonitrile yielding a white solid that was mixed with DMSO (13 mL) and water (12 mL). This mixture was heated minimally, filtered and to the filtrate was added TFA (0.25 mL) resulting in a precipitate. The precipitate was diluted with water (50 mL), filtered, washed with water and hexanes and dried on high vacuum yielding the title compound as a white solid (696 mg, 75%). ES(+)-LRMS m/e calcd. for C48H45F4N7O10 (M+H)+ 956, obsd 956.

1. concentrationThe reaction was concentrated
2. dry with materialdried from acetonitrile yielding a white solid that
3. additionwas mixed with DMSO (13 mL) and water (12 mL)
4. temperatureThis mixture was heated minimally
5. filtrationfiltered and to the filtrate
6. additionwas added TFA (0.25 mL)
7. customresulting in a precipitate
8. filtrationfiltered
9. washwashed with water and hexanes
10. customdried on high vacuum

ORDレコード

ord-f2ef8a99c1c5490bb0ac8a62f56ab6b3

出典データセット

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09447035B2