تفاعل #85933

معادلة التفاعل

water

2-(4-(6-fluoropyridin-2-yl)benzyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

hexachloroethane

LiHMDS

→

crude product

المردود 107.0%

3-chloro-2-(4-(6-fluoropyridin-2-yl)benzyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

المردود 107.0%

المذيبات

methylene chloride

THF

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with methylene chloride three times
2. 2
   أخرىThe combined organic phase is evaporated to dryness

الإجراء التجريبي

2-(4-(6-fluoropyridin-2-yl)benzyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (450 mg, 1.1 mmol) and hexachloroethane (523 mg, 2.2 mmol) are dissolved in 5 mL of methylene chloride, and then 1.0 M LiHMDS (2.2 mL, 2.2 mmol) in THF is added dropwise. After the reaction mixture is stirred at room temperature for 10 min, water is added, and then extracted with methylene chloride three times. The combined organic phase is evaporated to dryness to give 520 mg of crude product as off-white solids, which is used in the next step without further purification. MS (ESI) m/z 442.2 [M+H]+.

المصدر