反応 #58537

反応方程式

product

2-Benzyl-6,7-dimethyl-1,2,3,3a,7,7a-hexahydro-4-thia-2-aza-cyclopenta[α]pentalene

K2CO3

Ace-Cl

→

6,7-Dimethyl-1,2,3,3a,7,7a-hexahydro-4-thia-2-aza-cyclopenta[α]pentalene

溶媒

dichloroethane

反応条件

後処理

1. 1
   ろ過Next, the reaction mixture was filtered
2. 2
   濃縮concentrated
3. 3
   workup.DISSOLUTIONthe residue was dissolved in anhydrous MeOH (25 ml)
4. 4
   濃縮The MeOH was concentrated
5. 5
   その他triturated with ether producing 733 mg (95%) of the subtitle compound

実験手順

The product of step h) (948 mg, 3.35 mmol) in dichloroethane (17 ml) was treated with K2CO3 (1.85 g, 13.4 mmol) and Ace-Cl (1.45 ml, 13.4 mmol) at 80° C. for 16 hours. Next, the reaction mixture was filtered, concentrated and the residue was dissolved in anhydrous MeOH (25 ml) and stirred for 1 hour at 22° C. The MeOH was concentrated and triturated with ether producing 733 mg (95%) of the subtitle compound. 1H NMR (300 MHz, d6-DMSO, ppm) 1.27 (d, J=7 Hz, 3H); 2.97-3.10 (m, 1H); 3.19-3.38 (m, 2H); 3.42-3.62 (m, 3H); 3.78-3.88 (m, 1H); 6.92 (d, J=5 Hz, 1H); 7.47 (d, J=5 Hz, 1H); 9.05 (br s, 1H); 9.38 (br s, 1H); MS calculated for C11H15NS+H 194, observed 194.

出典