Sodium hydride → (5-Chlorothieno[2,3-d]pyrimidin-4-yl)-{2-[3-methoxy-4-(4-trifluoromethylpyridin-2-yloxy)phenyl]ethyl}amine

温度

80 °C

To a solution of 60 percent sodium hydride / oil dispersion (31 mg, 0.78 mmol) in DMSO (3 mL) was added 4-{2-[(5-chlorothieno[2,3-d]pyrimidin-4-yl)amino]ethyl}-2-methoxyphenol (250 mg, 0.75 mmol). After stirring for 30 min, 2-chloro-4-(trifluoromethyl)pyridine (141 mg, 0.78 mmol) was added and the reaction heated at 80° C. overnight. The reaction mixture was diluted with H2O and the precipitate collected by filtration. The filter cake washed with H2O and then dissolved in CH2Cl2. The organics were dried with (Na2SO4), filtered and the stripped in vacuo. The solid residue was triturated with a mixture of ether and pentane leaving a brown solid, 120 mg, 0.25 mmol, 33 percent yield.

1. filtrationthe precipitate collected by filtration
2. washThe filter cake washed with H2O
3. dissolutiondissolved in CH2Cl2
4. dry with materialThe organics were dried with (Na2SO4)
5. filtrationfiltered
6. customThe solid residue was triturated with a mixture of ether and pentane leaving a brown solid, 120 mg, 0.25 mmol, 33 percent yield

ORDレコード

ord-d8bd4739416f4aeeabad4d66d2a02228

出典データセット

uspto-grants-2009_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07531482B2