Hydrochloric Acid → 7-[4-(4-Fluorobenzoyl)benzyl]-5-methyl-2-methylthio-7H-pyrrolo[2,3-d]pyrimidin-4(3H)-one

温度

105 °C

Under argon gas, 7-[4-(4-fluorobenzoyl)benzyl]-4-methoxy-5-methyl-2-methylthio-7H-pyrrolo[2,3-d]pyrimidine (6.75 g) was dissolved in dioxane (45 ml) followed by addition of 4,4'-thiobis(6-t-butyl-m-cresol) (75 mg). Then, 0.5N-hydrochloric acid (12 ml) was added and the mixture was stirred at 105° C for 23 hours. Thereafter, 0.5N-hydrochloric acid (12 ml) was further added and the mixture was stirred at the same temperature as above for 22 hours. Then, 1N-hydrochloric acid (3 ml) and dioxane (6 ml) were added and the mixture was further stirred at the same temperature for 24 hours. This reaction mixture was allowed to stand at room temperature and the resulting crystals were collected by filtration, rinsed with methanol, DME, and ether, and finally dried to provide the title compound (5.35 g).

1. stirringthe mixture was stirred at the same temperature as above for 22 hours
2. stirringthe mixture was further stirred at the same temperature for 24 hours
3. customto stand at room temperature
4. filtrationthe resulting crystals were collected by filtration
5. washrinsed with methanol, DME, and ether
6. customfinally dried

ORDレコード

ord-add76740e4944b3ba794bcd45fa8a1f9

出典データセット

uspto-grants-1998_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05753664