1,2-Dimethoxyethane → HCID 18448299、化合物

温度

90 °C

A mixture of ethyl (4-{[(3-bromo-2-methylphenyl)(butyl)amino]methyl}-2-methylphenoxy)acetate (90 mg, 0.2 mmol), 4-methylphenylboronic acid (32 mg, 0.23 mmol), tetrakis(triphenylphosphine)palladium (0) (5 mg, 4.32 mmol), sodium carbonate (55 mg, 0.52 mmol) in 1,2-dimethoxyethane (10 mL) and water (5 mL) was heated at 90° C. for 18 h under nitrogen. The reaction mixture was cooled and the solvents removed in vacuo. Purification by SPE (C18, 10 g) eluting with 20 mL each of 5%, 10%, 30%, 50% acetonitrile/water, acetonitrile, MeOH. Further purification with SPE (amino propyl, 10 g), eluted with CH2Cl2 (40 mL), CHCl3 (20 mL), ether (20 mL), EtOAc (40 mL), MeOH (20 mL), 10% NH3/MeOH (40 mL) afforded the title compound as a colourless oil (50 mg).

1. temperatureThe reaction mixture was cooled
2. customthe solvents removed in vacuo
3. customPurification by SPE (C18, 10 g)
4. washeluting with 20 mL each of 5%, 10%, 30%, 50% acetonitrile/water, acetonitrile, MeOH
5. customFurther purification with SPE (amino propyl, 10 g)
6. washeluted with CH2Cl2 (40 mL), CHCl3 (20 mL), ether (20 mL), EtOAc (40 mL), MeOH (20 mL), 10% NH3/MeOH (40 mL)

ORDレコード

ord-20fb9d8d196c41499d8a1862d3c04a4d

出典データセット

uspto-grants-2007_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07199239B2