反应详情

温度

100 °C

To a stirred solution of (Z)-3-chloro-N′-hydroxybenzimidamide (500 mg, 2.93 mmol) and (S)-2-(1,3-dioxoisoindolin-2-yl)propanoic acid (642 mg, 2.93 mmol) was added N,N′-methanediylidenedicyclohexanamine (1.1 eq, 665 mg, 3.22 mmol) and allowed to reflux at 100° C. for 12 hours. Concentrate in vacuo, dilute w/EtOAc, filter washing w/EtOAc, wash w/water, brine, concentrate in vacuo. Flash column chromatography (silica, 40 g) eluting w/0-10% EtOAc/DCM afforded 300 mg. HRMS m/z 353.0567

1. concentrationConcentrate in vacuo
2. additiondilute w/EtOAc
3. filtrationfilter
4. washwashing
5. washwash w/water, brine
6. concentrationconcentrate in vacuo
7. washFlash column chromatography (silica, 40 g) eluting w/0-10% EtOAc/DCM
8. customafforded 300 mg