反応 #2267073

反応方程式

compound 11

3-Amino-4-methoxyphenylacetone

acetic anhydride

→

desired product 12

収率 97.0%

3-Acetylamino-4-methoxyphenylacetone

収率 97.0%

溶媒

chloroform

反応条件

後処理

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

実験手順

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).

出典