Morpholine → Morpholine, 4-(2-chloro-4-nitrophenyl)-

To a solution of morpholine (1.1 mL, 12.6 mmol) in DMF (30 mL) were added 2-chloro-1-fluoro-4-nitrobenzene (1.76 g, 10.0 mmol) and Et3N (4.2 mL, 30.1 mmol) with stirring and the mixture was stirred at rt overnight. The mixture was then filtered and the organic phase was poured into 150 mL of DCM, washed with water (150 mL×3) and brine (150 mL), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/DCM (V/V)=10:1) to give the title compound as a yellow solid (1.53 g, 63%).

1. stirringthe mixture was stirred at rt overnight
2. filtrationThe mixture was then filtered
3. additionthe organic phase was poured into 150 mL of DCM
4. washwashed with water (150 mL×3) and brine (150 mL)
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by a silica gel column chromatography (PE/DCM (V/V)=10:1)

ORDレコード

ord-f4072d50c2dc4c7bb60dd7a9c543384b

出典データセット

uspto-grants-2016_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09434695B2