反応 #443162

反応方程式

hydrochloric acid

ethyltrifluoroacetate

( 8 )

2,8-Diamino-6-fluoro-5-methyl-1-tetralone

ethanol

→

title compound

8-Amino-6-fluoro-5-methyl-2-trifluoroacetylamino-1-tetralone

溶媒

triethylamine

THF

反応条件

後処理

1. 1
   抽出extracted with chloroform
2. 2
   洗浄The extract was washed with water, saturated sodium bicarbonate and saturated brine in this order
3. 3
   乾燥dried over anhydrous sodium sulfate
4. 4
   その他After removal of the solvent
5. 5
   その他by evaporation
6. 6
   その他to obtain fractions
7. 7
   workup.ADDITIONcontaining the target compound
8. 8
   濃縮The fractions were concentrated

実験手順

The compound obtained in (8) above (1.66 gm) was dissolved into a mixed solvent of 70 ml of ethanol and 10 ml of THF. To the solution were added 2 ml of triethylamine and 1.5 ml of ethyltrifluoroacetate, followed by stirring for 20 hours at 20° C. The reaction product was added to dilute aqueous solution of hydrochloric acid and extracted with chloroform. The extract was washed with water, saturated sodium bicarbonate and saturated brine in this order, and dried over anhydrous sodium sulfate. After removal of the solvent by evaporation, the residue was subjected to silica gel column chromatography using chloroform as an eluant to obtain fractions containing the target compound. The fractions were concentrated to obtain 1.79 gm of the title compound.

出典