Potassium Carbonate → 3'-(4-chloro-phenyl)-4-(1,3-dimethyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2']bipyrazinyl

温度

110 °C

Add 4-chlorobenzeneboronic acid (64 mg, 0.41 mmol) to a mixture 3′-chloro-4-(1,3-dimethyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (104 mg, 0.34 mmol), potassium carbonate (113 mg, 0.82 mmol) and tetrakis(triphenylphosphine) palladium(0) (0.002 g, 0.002 mmol) in N,N-dimethylacetamide (2 mL) and water (1 mL). Purge with nitrogen and heat overnight at 110° C. Cool to room temperature add water (10 mL), extract with DCM (3×20 mL) combine and purify using high pH reverse phase HPLC to give 3′-(4-chloro-phenyl)-4-(1,3-dimethyl-1H-pyrazol-4-ylmethyl)-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl (68 mg, 54.2%). MS (ES): m/z=383 [M+H]+.

1. customPurge with nitrogen
2. temperatureCool to room temperature
3. additionadd water (10 mL)
4. extractionextract with DCM (3×20 mL) combine
5. custompurify

ORDレコード

ord-8b129fb1e82b43c48754a24d33e967c6

出典データセット

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08202873B2