Реакция #58559

ord-2996ca1e74824e76982146f3153ba8e9

Уравнение реакции

c1ccc(CN2CCC3c4sccc4CC3C2)cc1
product
c1ccc(CN2CCC3c4sccc4CC3C2)cc1
6-Benzyl-4,5,6,7,7a, 8-hexahydro-3bH-3-thia-6-aza-cyclopenta[α]indene
O=C([O-])[O-].[K+].[K+]
K2CO3
CC(Cl)OC(=O)Cl
Ace-Cl
c1cc2c(s1)C1CCNCC1C2
subtitle compound
Выход 94.0%
c1cc2c(s1)C1CCNCC1C2
4,5,6,7,7a,8-Hexahydro-3bH-3-thia-6-aza-cyclopenta[α]indene
Выход 94.0%

Растворители

Условия реакции

Температура
22°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияNext, the reaction mixture was filtered
  2. 2
    Концентрированиеconcentrated
  3. 3
    workup.DISSOLUTIONthe residue was dissolved in anhydrous MeOH (25 ml)
  4. 4
    КонцентрированиеThe MeOH was concentrated
  5. 5
    Другоеtriturated with ether

Методика

The product of step f) (1.16 g, 4.3 mmol) in dichloroethane (21 ml) was treated with K2CO3 (2.38 g, 17.2 mmol) and Ace-Cl (1.86 ml, 17.2 mmol) at 800C 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 to give 874 mg (94%) of the subtitle compound. MS calculated for C10H13NS+H 180, observed 180.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07423056B2uspto-grants-2008_09