Реакция #58555

ord-5e62bed0301d4377be51ee6ea4eb4aca

Уравнение реакции

c1ccc(CN2CCC3Cc4ccsc4C3C2)cc1
product
c1ccc(CN2CCC3Cc4ccsc4C3C2)cc1
5-Benzyl-4,5,6,7,7a,8-hexahydro-3bH-3-thia-5-aza-cyclopenta[α]indene
O=C([O-])[O-].[K+].[K+]
K2CO3
CC(Cl)OC(=O)Cl
Ace-Cl
c1cc2c(s1)C1CNCCC1C2
subtitle compound
Выход 66.0%
c1cc2c(s1)C1CNCCC1C2
4,5,6,7,7a,8-Hexahydro-3bH-3-thia-5-aza-cyclopenta[α]indene
Выход 66.0%

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 producing

Методика

The product from step f) (409 mg, 1.52 mmol) in dichloroethane (8 ml) was treated with K2CO3 (839 mg, 6.08 mmol) and Ace-Cl (658 μl, 6.08 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 to give 215 mg (66%) of the subtitle compound as its HCl salt. MS calculated for C10H13NS+H 180, observed 180.

Источник

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