Acetyl chloride → Acetamide, N-(2-methoxyphenyl)-

Temperature

2.5 °C

Ortho anisidine (0.67 moles, 82 g.) was taken in a 1 L round bottom flask equipped with a liquid addition funnel and a guard tube; triethylamine (1.0 mole, 100 g) was added to it in one lot. Above mixture was cooled to 0-5° C. and acetyl chloride was added drop-wise maintaining temperature below 10° C. After addition of acetyl chloride cooling was removed and the reaction mixture was stirred at 25-28° C. for 0.3 hours. After the completion of reaction (TLC), the reaction mixture was poured on ice-water, and aqueous layer was extracted with dichloromethane (2×300 mL). The combined dichloromethane extracts were then washed with water, brine and dried over anhydrous magnesium sulfate. The volatiles were removed under the reduced pressure to obtain 96.5 g. of solid.

1. customequipped with a liquid addition funnel and a guard tube
2. temperaturemaintaining temperature below 10° C
3. customwas removed
4. customAfter the completion of reaction (TLC)
5. additionthe reaction mixture was poured on ice-water, and aqueous layer
6. extractionwas extracted with dichloromethane (2×300 mL)
7. washThe combined dichloromethane extracts were then washed with water, brine
8. dry with materialdried over anhydrous magnesium sulfate
9. customThe volatiles were removed under the reduced pressure
10. customto obtain 96.5 g

ORD record

ord-8bb8c555e1da4862b4a9456a0aafc4c9

Source dataset

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07998981B2