Methanol → HCID 22316709、化合物

温度

0 °C

To a suspension of (3-methoxy-4-nitrophenyl)(methyl)sulfane (0.58 g, 2.9 mmol) in acetone (10 mL) was added water (10 mL), methanol (1.0 mL). The mixture was cooled in an ice-bath for 10 minutes before adding Oxone (2.90 g, 4.72 mmol) in four portions over 4 minutes. The reaction was stirred at 0° C. for 15 minutes and then allowed to warm up to room temperature. The reaction was stirred at room temperature for 2 hours before being diluted with EtOAc (50 mL). The suspension was filtered, concentrated to ⅓ of its volume and diluted with water (40 mL). The mixture was then extracted with EtOAc. The combined extracts were washed with brine, dried over sodium sulfate, filtered and concentrated to give 2-methoxy-4-(methylsulfonyl)-1-nitrobenzene (0.67 g, 83%).

1. temperatureThe mixture was cooled in an ice-bath for 10 minutes
2. temperatureto warm up to room temperature
3. stirringThe reaction was stirred at room temperature for 2 hours
4. filtrationThe suspension was filtered
5. concentrationconcentrated
6. additiondiluted with water (40 mL)
7. extractionThe mixture was then extracted with EtOAc
8. washThe combined extracts were washed with brine
9. dry with materialdried over sodium sulfate
10. filtrationfiltered
11. concentrationconcentrated

ORDレコード

ord-8dbaa5d0687941e181a169c5bcd4d899

出典データセット

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09145402B2