反应 #2267073

反应方程式

compound 11

3-Amino-4-methoxyphenylacetone

acetic anhydride

→

desired product 12

收率 97.0%

3-Acetylamino-4-methoxyphenylacetone

收率 97.0%

溶剂

chloroform

反应条件

后处理

1. 1
   其他The reaction was quenched
2. 2
   workup.ADDITIONby adding ice water
3. 3
   萃取extracted with CH2Cl2 twice
4. 4
   洗涤The organic layer was washed with brine
5. 5
   干燥dried over Na2SO4
6. 6
   其他Removal of the solvent
7. 7
   其他afforded the crude product
8. 8
   其他Purification of the crude product

实验过程

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).

来源