反応 #2286358

ord-94730d9d3bb0476fb0ae9e502f9a3e41

反応方程式

COc1ccc(P2(=S)SP(=S)(c3ccc(OC)cc3)S2)cc1
2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide
O=C(CC1CCCCC1)c1csc(C2CCN(C(=O)Cn3nc(C(F)F)cc3C(F)F)CC2)n1
2-[3,5-bis(difluoromethyl)-1H-pyrazol-1-yl]-1-{4-[4-(cyclohexylacetyl)-1,3-thiazol-2-yl]piperidin-1-yl}ethanone
O=C(CC1CCCCC1)c1csc(C2CCN(C(=S)Cn3nc(C(F)F)cc3C(F)F)CC2)n1
1-[2-(1-{2-[3,5-Bis(difluoromethyl)-1H-pyrazol-1-yl]ethanethioyl}piperidin-4-yl)-1,3-thiazol-4-yl]-2-cyclohexylethanone

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他After removal of the solvent under reduced pressure
  2. 2
    その他the residue was purified chromatographically

実験手順

At room temperature, 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (194 mg) was added to a solution of 2-[3,5-bis(difluoromethyl)-1H-pyrazol-1-yl]-1-{4-[4-(cyclohexylacetyl)-1,3-thiazol-2-yl]piperidin-1-yl}ethanone (200 mg) in toluene (2 ml). The reaction mixture was stirred at 60° C. for 2 hours. After removal of the solvent under reduced pressure, the residue was purified chromatographically. This gave 1-[2-(1-{2-[3,5-bis(difluoromethyl)-1H-pyrazol-1-yl]ethanethioyl}-piperidin-4-yl)-1,3-thiazol-4-yl]-2-cyclohexylethanone (101 mg, 49%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09357779B2uspto-grants-2016_06