반응 #2017241

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1,4-dioxaspiro[4.5]decane-8-carbonitrile

→

title compound

수율 23.0%

1,4-Dioxaspiro[4.5]decane-8-carbothioamide

수율 23.0%

용매

MeOH

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후처리

1. 1
   농축The mixture was concentrated under a stream of air
2. 2
   기타the resulting material was purified by flash chromatography on silica gel

실험 절차

The 1,4-dioxaspiro[4.5]decane-8-carbonitrile (1.16 g, 6.94 mmol, Tetrahedron, 2002, 58(8), 1557), ammonium sulfide (20 wt. % in water, 2.84 mL, 8.33 mmol) and MeOH (14 mL) were heated in a CEM® microwave at about 130° C. for about (250 psi maximum pressure, 10 min ramp, 300 max watts). The mixture was concentrated under a stream of air and the resulting material was purified by flash chromatography on silica gel using EtOAc/heptane (7:3) as an eluent to give the title compound (0.317 g, 23%) as a light yellow solid: LC/MS (Table 1, Method a) Rt=1.68 min; MS m/z: 202.1 (M+H)+.

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