Reacción #2267073

Ecuación de reacción

compound 11

3-Amino-4-methoxyphenylacetone

acetic anhydride

→

desired product 12

Rendimiento 97.0%

3-Acetylamino-4-methoxyphenylacetone

Rendimiento 97.0%

Disolventes

chloroform

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroThe reaction was quenched
2. 2
   workup.ADDITIONby adding ice water
3. 3
   Extracciónextracted with CH2Cl2 twice
4. 4
   LavadoThe organic layer was washed with brine
5. 5
   Secadodried over Na2SO4
6. 6
   OtroRemoval of the solvent
7. 7
   Otroafforded the crude product
8. 8
   OtroPurification of the crude product

Procedimiento

To the mixture of compound 11 (0.25 g, 1.39 mmol) in chloroform (30 ml) was added acetic anhydride (1.2 ml) and catalytic amount of DMAP (10 mg) at 0° C. After stirring at such temperature for 3 hours, no more starting materials were detected on TLC. The reaction was quenched by adding ice water, extracted with CH2Cl2 twice. The organic layer was washed with brine, dried over Na2SO4. Removal of the solvent afforded the crude product. Purification of the crude product by using silica gel column gave 0.3 g (97%) of desired product 12. 1HNMR(CDCl3): 8.25 (d, J=1.2 Hz, 1H), 7.79 (br, 1H), 6.81 (m, 2H), 3.86 (s, 3H), 3.64 (s, 2H), 2.20 (s, 3H), 1.95 (s, 3H).

Fuente