반응 #58566

반응 방정식

2-chloroethylchloroformate

K2CO3

product

7-Methyl-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[α]pentalene

→

HCl

subtitle compound

7-Methyl-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[α]pentalene

용매

methanol

반응 조건

후처리

1. 1
   workup.STIRRINGNext, the reaction was stirred for two hours at 75° C. after which the reaction mixture
2. 2
   온도was cooled
3. 3
   여과filtered
4. 4
   기타the solvent was evaporated
5. 5
   기타to leave an oily residue that
6. 6
   workup.STIRRINGwas stirred at room temperature for one hour
7. 7
   기타The solvent was evaporated
8. 8
   기타the residue was triturated in diethyl ether (5 mL)

실험 절차

K2CO3 (320 mg, 2.32 mmol) was added to a solution of the product from step g) (165 mg, 0.58 mmol) in 6 mL followed by the addition of 2-chloroethylchloroformate (332 mg, 2.32 mmol) under vigorous stirring at room temperature. Next, the reaction was stirred for two hours at 75° C. after which the reaction mixture was cooled, filtered and the solvent was evaporated to leave an oily residue that was then dissolved in dry methanol (10 mL) and was stirred at room temperature for one hour. The solvent was evaporated and the residue was triturated in diethyl ether (5 mL) to give the subtitle compound as its HCl salt. MS calculated for C10H13NS+H: 180, observed: 180. 1H NMR (CDCl3300 MHz) δ 1.32 (d, 3H), 1.93 (s, 1H), 3.04 (m, 1H), 3.18 (m, 2H), 3.47 (m, 3H), 3.78 (m, 1H), 6.83 (d, 1H), 7.21 (d, 1H) ppm.

출처