Potassium hydroxy sulfite → HCID 58541975、化合物

To a mixture of 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (135 mg, 0.53 mmol) and 2-(3-isopropyl-1,2,4-oxadiazol-5-yl)-benzaldehyde (139 mg, 0.64 mmol) in DMF (5.0 mL) is added Oxone (325 mg, 0.53 mmol) in H2O (2.0 mL). The reaction mixture is stirred at room temperature for 1 hour and then quenched with saturated sodium thiosulfate aq. (25 mL). The quenched reaction mixture is extracted with EtOAc (25 mL×2) and the combined organic layers are washed with H2O (50 mL×2) and dried with Na2SO4. The filtrate is concentrated under reduced pressure and the residue is purified by silica gel flash column chromatography with 3.5% MeOH in CH2Cl2 as the eluent to afford the title compound (105 mg, 44%) as a white solid. LCMS (ESMS): m/z 454.20 (M++1)

1. customquenched with saturated sodium thiosulfate aq. (25 mL)
2. customThe quenched reaction mixture
3. extractionis extracted with EtOAc (25 mL×2)
4. washthe combined organic layers are washed with H2O (50 mL×2)
5. dry with materialdried with Na2SO4
6. concentrationThe filtrate is concentrated under reduced pressure
7. customthe residue is purified by silica gel flash column chromatography with 3.5% MeOH in CH2Cl2 as the eluent

ORDレコード

ord-95d4ec40bc3341538c0d1a18a2bdc14d

出典データセット

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08420655B2